VERIFICATION OF THE DEFENSE WASTE PROCESSING …/67531/metadc...PROCESSING FACILITY’S (DWPF)...
Transcript of VERIFICATION OF THE DEFENSE WASTE PROCESSING …/67531/metadc...PROCESSING FACILITY’S (DWPF)...
SRNL-STI-2011-00475, REVISION 0
VERIFICATION OF THE DEFENSE WASTE
PROCESSING FACILITY’S (DWPF) PROCESS
DIGESTION METHOD FOR THE SLUDGE BATCH 7B
BLEND SAMPLE
D. R. Click
T. B. Edwards
B.J. Wiedenman
August 29, 2011
Analytical Development
Savannah River National Laboratory
Aiken, SC 29808
Prepared for the U.S. Department of Energy Under Contract Number
DE-AC09-08SR22470
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DISCLAIMER
This work was prepared under an agreement with and funded by the U.S.
Government. Neither the U.S. Government or its employees, nor any of its
contractors, subcontractors or their employees, makes any express or implied:
1. warranty or assumes any legal liability for the accuracy, completeness, or for the use
or results of such use of any information, product, or process disclosed;
2. representation that such use or results of such use would not infringe privately
owned rights; or
3. endorsement or recommendation of any specifically identified commercial product,
process, or service. Any views and opinions of authors expressed in this work do not
necessarily state or reflect those of the United States Government, or its contractors, or
subcontractors.
Printed in the United States of America
Prepared For
U.S. Department of Energy
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Key Words: method development,
analytical process, SB7,
waste compliance
Retention:
Permanent
VERIFICATION OF THE DEFENSE WASTE
PROCESSING FACILITY’S (DWPF) PROCESS
DIGESTION METHOD FOR THE SLUDGE BATCH 7B
BLEND SAMPLE
D. R. Click
T. B. Edwards
B.J. Wiedenman
August 29, 2011
Analytical Development
Savannah River National Laboratory
Aiken, SC 29808
Prepared for the U.S. Department of Energy Under Contract Number
DE-AC09-08SR22470
SRNL-STI-2011-00475, REVISION 0
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REVIEWS AND APPROVALS ______________________________________________________________________________ D.R. Click, Author, Analytical Development, SRNL Date ______________________________________________________________________________ T.B. Edwards, C-Author, ACES, SRNL Date ______________________________________________________________________________ B.J. Wiedenman, Co-Author, Analytical Development, SRNL Date ______________________________________________________________________________ D.P. Lambert, Technical Reviewer, E&CTP Research Programs, SRNL Date ______________________________________________________________________________ C.C. Herman, Manager, DWPF Programs, SRNL Date ______________________________________________________________________________ C.M Gregory, Manager, Spectroscopy and Separations, Analytical Development, SRNL Date ______________________________________________________________________________ J.E. Occhipinti, Manager, Waste Solidification Engineering, SRR Date
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VII
TABLE OF CONTENTS
0HLIST OF AND FIGURES AND TABLES ................................................................................... IX LIST OF ACRONYMS ................................................................................................................. XI 1.0 0BSUMMARY ......................................................................................................................... 13 2.0 1BEXPERIMENTAL ............................................................................................................... 15 3.0 2BINTRODUCTION AND RESULTS ................................................................................... 17 4.0 3BCONCLUSIONS ................................................................................................................. 29 5.0 4BRECOMMENDATIONS ..................................................................................................... 31 6.0 5BREFERENCES .................................................................................................................... 33 7.0 6BACKNOWLEDGEMENTS ................................................................................................. 35 8.0 7BAPPENDIX A. SUPPORTING INFORMATION ............................................................. 37
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LIST OF AND FIGURES AND TABLES
10HTable 3-1. Elemental concentrations of SB7b SRAT Receipt radioactive sludge slurry obtained from ICP-AES
analysis of Aqua Regia, DWPF Cold Chem method and Sodium Peroxide/Hydroxide Fusion digestions.
Values are presented on a weight percent (wt%) of total dried solids basis................................................ 19 Table 3-2 Statistical comparison of Aqua Regia, DWPF Cold Chem method and Sodium Peroxide/Hydroxide
Fusion digestions of SB7b SRAT Receipt sludge. Digestion methods not having similar bold font or those
that are not underlined are statistically different at the 5% significance level. The less than sign indicates
the digestion method with the lowest and highest mean concentration from ICP-AES measurements. ..... 20 Table 3-3. Elemental concentrations of SB7b SRAT Product radioactive sludge slurry obtained from ICP-AES
analysis of Aqua Regia, DWPF Cold Chem method and Sodium Peroxide/Hydroxide Fusion digestions.
Values are presented on a weight percent (Wt%) total dried solids basis. .................................................. 21 Table 3-4. Statistical comparison of Aqua Regia, DWPF Cold Chem method and Sodium Peroxide/Hydroxide
Fusion digestions of SB7b SRAT Product sludge. Digestion methods not having similar bold font or those
that are not underlined are statistically different at the 5% significance level. ........................................... 22 Table 3-5. Elemental concentrations of ARG standard from ICP-AES analysis of Aqua Regia, and Sodium
Peroxide/Hydroxide Fusion digestions performed concurrently with SB7b SRAT Receipt Sample. Values
are presented on a weight percent (Wt%) total solids basis. ....................................................................... 24 Table 3-6. E concentrations of ARG standard from ICP-AES analysis DWPF Cold Chem method digestions
performed concurrently with SB7b SRAT Receipt Sample. Values are presented on a weight percent
(Wt%) total solids basis. ............................................................................................................................. 25 Table 3-7. Elemental concentrations of ARG standard from ICP-AES analysis of Aqua Regia, and Sodium
Peroxide/Hydroxide Fusion digestions performed concurrently with SB7b SRAT Product sample. Values
are presented on a weight percent (Wt%) total solids basis. ....................................................................... 26 Table 3-8. Continuation of elemental concentrations of ARG standard from ICP-AES analysis of Aqua Regia,
DWPF Cold Chem method and Sodium Peroxide/Hydroxide Fusion digestions performed concurrently
with SB7b SRAT Product sample. Values are presented on a weight percent (Wt%) total solids basis..... 27
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XI
LIST OF ACRONYMS
AD Analytical Development
AR Aqua Regia
ARG Analytical Reference Glass
CC Cold Chem
DI De-Ionized
DOE Department of Energy
DWPF Defense Waste Processing Facility
ICP-AES Inductively Coupled Plasma – Atomic Emission Spectroscopy
LWO Liquid Waste Operations
PF Sodium Peroxide/Hydroxide Fusion
SB Sludge Batch
SME Slurry Mix Evaporator
SRAT Sludge Receipt and Adjustment Tank
SRNL Savannah River National Laboratory
WAPS Waste Acceptance Product Specification
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1.0 0BSUMMARY
For each sludge batch that is processed in the Defense Waste Processing Facility (DWPF), the Savannah
River National Laboratory (SRNL) performs confirmation of the applicability of the digestion method to
be used by the DWPF lab for elemental analysis of Sludge Receipt and Adjustment Tank (SRAT) receipt
samples and SRAT product process control samples. DWPF SRAT samples are typically dissolved using
a room temperature HF-HNO3 acid dissolution (i.e., DWPF Cold Chem Method, see DWPF Procedure
SW4-15.201) and then analyzed by inductively coupled plasma – atomic emission spectroscopy (ICP-
AES).
This report contains the results and comparison of data generated from performing the Aqua Regia (AR),
Sodium Peroxide/Hydroxide Fusion (PF) and DWPF Cold Chem (CC) method digestions of Sludge Batch
7b (SB7b) SRAT Receipt and SB7b SRAT Product samples. The SB7b SRAT Receipt and SB7b SRAT
Product samples were prepared in the SRNL Shielded Cells, and the SRAT Receipt material is
representative of the sludge that constitutes the SB7b Blend, the sludge expected to be in Tank 40.
Observations and results from the SRAT Receipt digestions include the following:
Brown/red solids and white solids remained in the solutions generated from the CC digestion
after all acid addition steps and dilutions were performed. The brown/red colored solids
eventually dissolved.
A statistically larger average Al concentration is seen in the PF digestions compared
to the AR and CC methods with an ~3% and an ~6% relative difference in the means,
respectively.
There is not a statistical difference in the means for Th between the AR and PF digestion results
but a statistical difference in the means is noted between the mean of the CC digestions and the
AR and PF means with an ~22% and an ~16% relative difference in the means, respectively.
A statistical difference in the means is noted for U between the PF results compared to the AR
and CC results. The PF mean is ~5% lower than the AR results and ~7% lower than the CC
result.
A statistical difference of means is noted for the minor elements Cr, Cu, K, Li, Mg, Ti and Zr
between two or more of the digestion methods.
There is not a statistical difference in the means for Fe, Mn, or Ni, nor is there a statistical
difference in the mean Na concentration obtained by the AR and CC digestion methods.
Observations and results from the SRAT Product digestions include the following:
Brown/red solids and white solids remained in the solutions generated from the CC digestion
after all acid addition steps and dilutions were performed. The brown/red colored solids
eventually dissolved.
A statistically larger average Al concentration is seen in the PF digestions compared
to the AR and CC methods with an ~2% and an ~7% relative difference in the means,
respectively.
There is not a statistical difference in the means for Th between the AR and PF digestion results
but a statistical difference in the means is noted between the mean of the CC digestions and the
AR and PF means with an ~26% and an ~18% relative difference in the means, respectively.
A statistical difference of means is noted for the minor elements Cu, K, Ti and Zr between two or
more of the digestion methods.
There is not a statistical difference in the means for Cr, Fe, Li, Mg, Mn, Ni, or U, nor is there a
statistical difference in the mean Na concentration obtained by the AR and CC digestion methods.
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Based on the results from performing three different digestion methods on SB7b sludge slurry, SRNL
notes and recommends the following:
The results from using the DWPF CC method to digest SB7b sludge slurry appear, in most cases,
to be equivalent to the AR and PF digestion methods. However, Al and Th should be analyzed by
the peroxide fusion method for SB7b. Visual observations indicate Fe and Mn may not be
completely dissolving in the initial dilution of the sample before the final dilution is performed.
For this data set, very small relative differences between the digestion methods are noted and no
statistical difference is observed between the digestion methods for Fe and Mn. However, we
recommend that the Fe and Mn concentration be determined using both digestion methods (CC
and PF) for SB7b sludge slurry and the highest concentration between the two digestions should
be used. Although K is a minor element, large relative differences are noted in this report between
the different digestions and the DWPF should also monitor the K concentration.
The DWPF CC method was originally developed to be used for SME analyses. Given continuous
visual observations of solids in the CC digestions both at SRNL and DWPF, potential issues with
accurate Al measurements when processing HM waste, and difficulty measuring Th accurately
due to the limited solubility of Th in HF matrices, SRNL recommends that the DWPF consider a
different digestion scheme that relieves some of these issues.
The DWPF CC results from this study indicate Al and Th do not completely dissolve or
precipitate as fluoride salts. Visual observations also indicate Fe and Mn may not
completely dissolve using the DWPF CC method. Therefore, DWPF should consider and
monitor the impact of these elements on SB7b blending operations conducted at DWPF
via comparison of SRAT and SME analyses. If a consistent difference in elemental
concentrations is revealed, another type of digestion (i.e. sodium peroxide/hydroxide fusion)
should be used to determine the concentration of the element in question. Particular emphasis
should be placed on monitoring Al, Fe, Mn, K, and Th concentrations in SB7b.
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2.0 1BEXPERIMENTAL
The SB7b sample used for this study was the SB7b SRAT Receipt sample comprised of the following;
Tank 7 sludge from sample FTF-07-11-3, Tank 51 sludge from sample HTF-51-11-28 (the Sludge Batch
7a confirmation sample), H Canyon Pu solution, and a salt solution were combined to produce a slurry
with a composition to match Tank Farm projections of April 27, 2011. The material was not in the
multiple steps washed as the Tank Farm would wash due to schedule constraints; instead, one "Wash",
using the salt solution, was used to produce the slurry. Then, the Tank 7/Tank 51 mixture was combined
with the Sludge Batch 7a Tank 40 Waste Acceptance Product Specification sample (HTF-40-11-66) to
produce the SB7b. The blended sample was 71% Tank 40, 29% Tank 7/Tank 51 measured on an
insoluble solids basis. The blend represented the highest projected Tank 40 heel (as of May 25, 2011) for
the planned SB7b transfer.
The sludge samples were dissolved in quadruplicate in the SRNL Shielded Cells facility in a manner
similar to the DWPF CC method, and by PF and AR digestion. For detailed steps of the PF digestion, see
ADS procedure 2502.1 For detailed steps of the AR digestion, see ADS procedure 2226.
2 Three replicate
dissolutions of the analytical reference glass (ARG) standard were performed concurrently with each set
of digestions for quality control purposes. The ARG results are then evaluated by comparing the
measured results against a two sigma variation of the standard deviation associated with measured
concentrations obtained from a round-robin consensus study. For the SRAT Receipt material, B, Si, Ti,
and Zr (as expected) were low and flagged for being outside of the 2 sigma limits for the AR digestions.
Ca was flagged for being outside the 2 sigma limits (slightly high) for the PF digestions. Ca and Fe were
flagged for being outside the 2 sigma limits (slightly high) for the CC digestions. For the SRAT product
material, Al, B, Si, Ti and Zr (as expected) were flagged for being outside of the 2 sigma limits for the
AR digestions. All elements were within the 2 sigma limits for the CC digestions. Ca was flagged for
being outside of the 2 sigma limits for the PF digestions. Additional quality control measures included
ICP-AES analyses of a multi-element standard as a check for ICP-AES accuracy independent of
digestions. Elements in this standard included Al, Fe, Mn, Ni, Na and S. All measured values were
within 15% of the known concentrations for these elements in the standard analyzed concurrently with the
PF and AR digestions.
The CC method digestion (see DWPF Procedure SW4-15.201) involved adding 25 mL of concentrated
HF to radioactive sludge slurry (~3.5 g for the SRAT Receipt at 16.05 wt% total solids and ~3.5 g for the
SRAT Product at 23.6 wt% total solids) and stirring for 1 hr. Then, 25 mL of concentrated HNO3 was
added and the mixture was stirred for an additional 30 minutes. Undissolved brown/red solids remained
in each digestion bottle after the acid addition was complete. Each sample was then diluted with de-
ionized (DI) water to 250 mL in a pre-weighed volumetric flask. The density of the solution was obtained
from the weight of the 250 mL of solution. Approximately 15 g of solution was taken from the 250 mL
volumetric flask and added to a 100 mL volumetric flask and subsequently diluted with DI water. Over
time, all of the brown solids dissolved into the solution but white insoluble/precipitated solids remained.
No attempt to recover the solids was made.
.
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3.0 2BINTRODUCTION AND RESULTS
The DWPF is currently processing and immobilizing radioactive sludge slurry into a durable borosilicate
glass. The DWPF has already processed seven sludge batches (Sludge Batch 1A, Sludge Batch 1B,
Sludge Batch 2, Sludge Batch 3, Sludge Batch 4, Sludge Batch 5, Sludge Batch 6) and is currently
processing an eighth (Sludge Batch 7a). A sludge batch is defined as a single tank of sludge or a
combination of sludges from different tanks that has been or will be qualified before being transferred to
DWPF. Thus, following the sludge batch preparation plan of the Liquid Waste Organization (LWO), the
qualified sludge in Tank 51 is to be blended with the heel of the previous sludge batch in Tank 40
(referred to as a “blend” composition in sludge batch planning). The sludge being qualified at the SRNL
is the “blend” sample, a sludge sample that has been blended with Tank 40 material representing the heel
of the previous sludge batch. The next batch of radioactive sludge slurry to be processed by the DWPF is
SB7b.
The statistical results of the SB7b samples generated from this study are provided in Table A1 of
Appendix A. The results from each type of digestion are summarized in 36HTable 3-1 for the SRAT Receipt
and Table 3-3 for the SRAT Product samples. The ICP-AES results of the seventeen elements that are
analyzed by the DWPF lab are presented on a weight percent (wt%) of total solids basis. A statistical
comparison of the means from the SRAT Receipt and SRAT Product for all three digestions could not be
performed for B, Ca, Na, Si or Zr. B was less than the detection limit in the AR and PF digestions and B
is leached from the borosilicate spray chamber of the ICP-AES instrument due to the presence of HF in
the CC digestions and is therefore not reported. Ca is a contaminant in the PF reagents and is not
included in the means with the AR and CC digestions for comparison. Na is added as part of the reagents
used for PF digestions so only the means of the CC and AR digestions were compared. Si is leached from
the ICP-AES instrument due to the presence of HF in the CC digestions and Si is known to not dissolve
well in AR digestions. Thus, the Si value obtained from the PF data was used. Zr could not be included
in a statistical comparison of all the means because the PF digestion utilizes a Zr crucible; therefore, only
the AR and CC results were compared. However, the Zr result from the AR digestions was low. Zr
dissolves better when HF is present and this can readily be seen from the ARG-1 analysis results. In
addition, for the SRAT Receipt, the K concentrations could not be compared because K was less than the
minimum detection limit in all three digestions and for the SRAT product sample, the potassium
concentration was less than the minimum detection limit in the CC digestion solutions.
Statistical comparisons of the data from the three digestion methods (for B, Na, Si and Zr there are only
two digestion methods) are provided in Exhibit A1 in Appendix A. The results were generated using
JMP Version 7.0.2.3 The plots of this exhibit show a 95% confidence interval for the mean (a mean
diamond) of each set of measurements. For each element, the mean concentration of the samples by each
digestion method is provided, and means that are not connected by the same letter in the listing of the
exhibit are significantly different at a significance level of 5%. For example, consider the SRAT Receipt
Al measurements. The results of the exhibit indicate that the mean of the PF results differs from the mean
of the CC results. The exhibit also indicates the means for the CC results and the AR results are not
statistically different and the means from the AR results and the PF results are not statistically different.
For the B, Na, Si, Zr comparisons, the JMP output from an analysis of variance of the measurements for
two digestions is provided, and only the 95% confidence mean diamond of each digestion is shown.
Overlap marks show for each diamond, and overlap marks in one diamond that are closer to the mean of
another diamond than that diamond's overlap marks indicate that those two groups are not different at the
95% confidence level. The visual comparisons are supported by an F test that compares the means of the
AR and CC digestions for Na and Zr and the means of the AR and PF digestions for B and Si. If the p
value is less than 0.05, then the means are statistically different at the 5% level. From Exhibit A1, there is
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no statistical difference in the AR and CC means for Na for the SRAT Product or the SRAT Receipt
samples.
Summaries of the statistical comparisons of Exhibit A1 are shown in Table 3-2 and Table 3-4.
Digestion methods not having the same bold font or those that are not underlined are statistically
different at the 5% significance level. The less than sign indicates the digestion method with the
lowest and highest mean concentration from ICP-AES measurements. Tables 3-5 through 3-8
contain the ARG-1 digestion results from the three digestion methods with a relative comparison to the
known concentration of specific elements in the ARG-1 glass.
During verification of the DWPF CC method for previous sludge batches, boehmite (AlO(OH)),
muscovite (K,Na)(Al, Mg, Fe)2(Si3.1Al0.9)O10(OH)2, silicon dioxide (SiO2), dipotassium sodium aluminum
fluoride (K2NaAl3F12), dipotassium aluminum pentafluoride (K2AlF5), aluminum fluoride (AlF3), chiolite
(Na5Al3F14), cryolite (Na3AlF6), sodium magnesium aluminum hexafluoride (NaMgAlF6), iron zirconium
hexafluoride (FeZrF6), disodium iron aluminum heptafluoride (Na2FeAlF7), and calcium thorium fluoride
(Ca0.5Th0.5F3) have been found.4 Due to the radioactivity of the samples, no attempt to recover the solids
was made.
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Table 3-1. Elemental concentrations of SB7b SRAT Receipt radioactive sludge slurry obtained from ICP-
AES analysis of Aqua Regia, DWPF Cold Chem method and Sodium Peroxide/Hydroxide Fusion digestions.
Values are presented on a weight percent (wt%) of total dried solids basis.
Digestion
Method →
Aqua Regia Na2O2/NaOH
Fusion
DWPF Cold Chem
Element Avg Wt% %RSD# Avg Wt% %RSD
# Avg Wt% %RSD
#
Al 8.48E+00 3.8E+00 8.83E+00 3.0E-01 8.14E+00 2.6E+00
B <8.17E-03 NA <8.10E-02 NA NA NA
Ca 6.38E-01 4.7E+00 7.53E-01 2.5E+00 6.62E-01 1.7E+00
Cr 4.31E-02 5.8E+00 6.04E-02 2.2E+01 4.44E-02 2.6E+00
Cu 8.00E-02 5.2E+00 4.87E-02 5.6E+00 4.44E-02 6.7E-01
Fe 1.42E+01 4.5E+00 1.43E+01 1.5E-14 1.45E+01 3.5E-01
K <2.58E-02 NA <2.56E-01 NA <1.89E-01 NA
Li 2.65E-02 5.6E+00 2.34E-02 2.5E+00 2.50E-02 1.7E+00
Mg 2.85E-01 4.8E+00 2.77E-01 9.6E-01 2.96E-01 3.2E-01
Mn 3.02E+00 4.8E+00 2.98E+00 3.4E-01 3.12E+00 3.1E-01
Na 1.41E+01 4.5E+00 NA NA 1.46E+01 3.4E-01
Ni 2.94E+00 4.6E+00 2.95E+00 3.9E-01 2.98E+00 3.4E-01
Si 4.72E-01 1.9E+01 1.06E+00 5.5E-01 NA NA
Th 1.04E+00 4.8E+00 9.56E-01 3.2E+00 7.61E-01 9.6E+00
Ti 1.69E-02 5.2E+00 1.97E-02 7.8E-01 1.93E-02 7.4E+00
U 4.77E+00 3.7E+00 4.45E+00 1.3E+00 4.98E+00 5.7E-01
Zr 1.39E-01 1.7E+01 NA NA 2.70E-01 8.8E-01
Averages are based upon four replicate dissolutions and ICP-AES determinations except the Peroxide Fusion
averages which are based upon three replicate dissolutions and ICP-AES measurements. NA = Not Applicable. #%RSD is the percent relative standard deviation for the measurements.
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Table 3-2 Statistical comparison of Aqua Regia, DWPF Cold Chem method and Sodium Peroxide/Hydroxide
Fusion digestions of SB7b SRAT Receipt sludge. Digestion methods not having similar bold font or those that
are not underlined are statistically different at the 5% significance level. The less than sign indicates the
digestion method with the lowest and highest mean concentration from ICP-AES measurements.
Statistical
Comparisons Element
Al CC < AR < PF
B# NA
Ca AR < CC
Cr AR < CC < PF
Cu CC < PF < AR
Fe AR < PF < CC
K#
NA
Li PF < CC < AR
Mg PF < AR < CC
Mn PF < AR < CC
Na AR < CC
Ni AR < PF < CC
Si AR < PF
Th CC < PF < AR
Ti AR < CC <PF
U PF < AR < CC
Zr AR < CC #Below ICP-AES detection levels, less than values reported.
For the SRAT Receipt sample:
Brown/red solids and white solids remained in the solutions generated from the CC digestion
after all acid addition steps and dilutions were performed. The brown/red colored solids
eventually dissolved.
A statistically larger average Al concentration is seen in the PF digestions compared
to the AR and CC methods with an ~3% and an ~6% relative difference in the means,
respectively.
There is not a statistical difference in the means for Th between the AR and PF digestions but a
statistical difference in the means is noted comparing CC digestions to the AR and PF means with
an ~22% and an ~16% relative difference in the means, respectively.
A statistical difference in the means is noted for U between the PF results compared to the AR
and CC results. The PF results are ~5% lower than the AR results, and ~7% lower than the CC
results.
A statistical difference of means is noted for the minor elements Cr, Cu, K, Li, Mg, Ti and Zr.
There is not a statistical difference in the means for Fe, Mn, or Ni, nor is there a statistical
difference in the mean Na concentration from the AR and CC digestions.
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40HTable 3-5 through 41HTable 3-8 contain the ICP-AES measured weight percent elemental results from
digestion of the ARG standard performed concurrently with the SB7b SRAT samples to determine if the
dissolutions were complete and the resulting analyses accurate. A statistical comparison of means from
the results of digesting the glass standard (ARG-1) by all three methods was not performed due to the
small number of observations. However, relative differences are listed in Tables 3-5 through 3-8. For the
AR digestions, Cu and Ti were the only elements with a relative difference greater than 10% compared to
the known concentration of Cu and Ti in the ARG-1 standard. The Cu concentration reported was close
to the ICP-AES detection limit which explains the large relative difference. Si and Zr are not considered
because the means of these elements are expected to be greater than 10% different. For the PF digestions,
the Ca and Cr means were greater than 10% different than the known concentrations in ARG-1. Ca is a
contaminant in the PF reagents. For the CC digestions, Ca, Cr, and Cu had means greater than 10%
different than the known concentrations in ARG-1 standard.
Table 3-3 contains the elemental concentrations of the SB7b SRAT Product sample.
Table 3-3. Elemental concentrations of SB7b SRAT Product radioactive sludge slurry obtained from ICP-
AES analysis of Aqua Regia, DWPF Cold Chem method and Sodium Peroxide/Hydroxide Fusion digestions.
Values are presented on a weight percent (Wt%) total dried solids basis.
Digestion
Method →
Aqua Regia Na2O2/NaOH
Fusion
DWPF Cold Chem
Element Avg Wt%* %RSD# Avg Wt%* %RSD
# Avg Wt%* %RSD
#
Al 7.65E+00 2.9E+00 8.49E+00 1.3E+00 8.22E+00 5.7E+00
B <7.97E-03 NA <1.74E-02 NA NA NA
Ca 6.13E-01 4.0E+00 7.60E-01 5.3E+00 6.20E-01 4.6E+00
Cr 4.08E-02 4.3E+00 4.56E-02 3.0E+00 4.49E-02 7.0E+00
Cu 4.03E-02 3.9E+00 4.36E-02 1.7E+00 4.00E-02 4.3E+00
Fe 1.37E+01 3.5E+00 1.36E+01 8.2E-01 1.38E+01 5.3E+00
K 5.51E-02 5.1E+00 2.89E-01 1.3E+01 <1.29E-01 NA
Li 2.53E-02 4.3E+00 2.50E-02 4.2E+00 2.65E-02 7.4E+00
Mg 2.78E-01 3.9E+00 2.74E-01 1.3E+00 2.93E-01 4.9E+00
Mn 2.94E+00 3.6E+00 2.97E+00 1.0E+00 3.02E+00 5.2E+00
Na 1.49E+01 3.7E+00 NA NA 1.51E+01 4.8E+00
Ni 2.81E+00 3.6E+00 2.76E+00 1.0E+00 2.82E+00 5.2E+00
Si 4.21E-01 1.9E+01 1.07E+00 1.0E+00 NA NA
Th 1.06E+00 3.7E+00 9.39E-01 5.5E+00 7.27E-01 1.3E+01
Ti 1.58E-02 3.7E+00 1.90E-02 2.4E+00 1.49E-02 2.5E+00
U 4.48E+00 3.7E+00 4.26E+00 3.0E+00 4.51E+00 4.0E+00
Zr 1.50E-01 1.2E+01 NA NA 2.54E-01 6.1E+00
*Averages are based upon four replicate dissolutions and ICP-AES determinations except the Peroxide Fusion
averages which are based upon three replicate dissolutions and ICP-AES measurements. NA = Not Applicable.. #%RSD is the percent relative standard deviation for the measurements
A statistical comparison of means from SB7b SRAT product digestions is presented in Table 3-4.
SRNL-STI-2011-00475, REVISION 0
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Table 3-4. Statistical comparison of Aqua Regia, DWPF Cold Chem method and Sodium Peroxide/Hydroxide
Fusion digestions of SB7b SRAT Product sludge. Digestion methods not having similar bold font or those that
are not underlined are statistically different at the 5% significance level. The less than sign indicates the
digestion method with the lowest and highest mean concentration from ICP-AES measurements.
Statistical
Element Comparisons
Al AR < CC < PF
B# NA
Ca AR < CC
Cr AR < CC < PF
Cu CC < AR < PF
Fe PF < AR < CC
K AR < PF
Li PF < AR < CC
Mg PF < AR < CC
Mn AR < PF < CC
Na AR < CC
Ni PF < AR < CC
Si AR < PF
Th CC < PF < AR
Ti CC < PF < AR
U PF < AR < CC
Zr AR < CC
#Below ICP-AES detection levels, less than values reported.
Observations and results from the SRAT Product digestions include the following:
Brown/red solids and white solids remained in the solutions generated from the CC digestion
after all acid addition steps and dilutions were performed. The brown/red colored solids
eventually dissolved.
A statistically larger average Al concentration is seen in the PF digestions compared
to the AR and CC methods with an ~2% and an ~7% relative difference in the means,
respectively.
There is not a statistical difference in the means for Th between the AR and PF digestions but a
statistical difference in the means is noted comparing the CC digestions to the AR and PF means
with an ~26% and an ~18% relative difference in the means, respectively.
A statistical difference of means between the three digestion methods is noted for the minor
elements Cu, K, Ti and Zr.
There is not a statistical difference in the means for Cr, Fe, Li, Mg, Mn, Ni, or U, nor is there a
statistical difference in the mean Na concentration from the AR and CC digestions.
SRNL-STI-2011-00475, REVISION 0
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The ARG digestions results are as follows. For the AR digestions, the mean B, (slightly low) Cu, and Ti
results differed by more than 10% from the known concentration in the ARG-1 standard. Si and Zr are
not considered because the mean results from of these elements are expected to be greater than 10%
different. For the PF digestions, B, Ca and Cr means were greater than 10% different from than the
known concentrations in ARG-1. Ca is a contaminant in the PF reagents. For the CC digestions, the
measured Cu concentration differed by more than 10% from the known concentration, most likely
because the concentration in the solutions is very near the ICP-AES detection limit which is reflected by
the high %RSD reported with the measurement.
SRNL-STI-2011-00475, REVISION 0
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Table 3-5. Elemental concentrations of ARG standard from ICP-AES analysis of Aqua Regia, and Sodium
Peroxide/Hydroxide Fusion digestions performed concurrently with SB7b SRAT Receipt Sample. Values are
presented on a weight percent (Wt%) total solids basis.
Aqua Regia
Element Average
Wt%
%RSD – only one
Standard
Analyzed
Standard Value %Difference
(Measured vs
Standard Value)
Al 2.35E+00 NA 2.50E+00 -6.0
B 2.43E+00 NA 2.69E+00 -9.7
Ca 9.86E-01 NA 1.02E+00 -3.3
Cr 6.74E-02 NA 6.40E-02 5.3
Cu 5.44E-03 NA 3.00E-03 81.3
Fe 9.39E+00 NA 9.79E+00 -4.1
K 2.26E+00 NA 2.26E+00 0.0
Li 1.40E+00 NA 1.49E+00 -6.0
Mg 5.17E-01 NA 5.20E-01 -0.6
8BMn 1.47E+00 NA 1.46E+00 0.7
Na 8.06E+00 NA 8.52E+00 -5.4
Ni 8.00E-01 NA 8.27E-01 -3.3
Si 9.99E-01 NA 2.24E+01 -95.5
Ti 6.17E-01 NA 6.90E-01 -10.6
Zr 2.57E-02 NA 9.60E-02 -73.2
Sodium Peroxide/Hydroxide Fusion
Element Average
Wt%
%RSD – only one
Standard
Analyzed
Standard Value %Difference
(Measured vs
Standard Value)
Al 2.59E+00 NA 2.50E+00 3.6
B 2.52E+00 NA 2.69E+00 -6.3
Ca 1.20E+00 NA 1.02E+00 17.6
Cr 7.09E-02 NA 6.40E-02 10.8
Cu <5.04E-03 NA 3.00E-03 NA
Fe 9.97E+00 NA 9.79E+00 1.8
K 2.32E+00 NA 2.26E+00 2.7
Li 1.50E+00 NA 1.49E+00 0.7
Mg 5.33E-01 NA 5.20E-01 2.5
Mn 1.48E+00 NA 1.46E+00 1.4
Na NA NA 8.52E+00 NA
Ni 8.54E-01 NA 8.27E-01 3.3
Si 2.24E+01 NA 2.24E+01 0.0
Ti 7.10E-01 NA 6.90E-01 2.9
Zr NA NA 9.60E-02 NA
NA = Not applicable. <MDL = less than minimum detection limit.
\
SRNL-STI-2011-00475, REVISION 0
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Table 3-6. E concentrations of ARG standard from ICP-AES analysis DWPF Cold Chem method digestions
performed concurrently with SB7b SRAT Receipt Sample. Values are presented on a weight percent (Wt%)
total solids basis.
DWPF Cold Chem Method*
Element Average %RSD Known Value %Difference
(Measured vs
Known Value)
Al 2.58E+00 2.2E+00 2.50E+00 3.2
B NA NA 2.69E+00 NA
Ca 1.13E+00 1.3E+00 1.02E+00 10.8
Cr 7.29E-02 1.8E+00 6.40E-02 13.8
Cu 3.77E-03 2.2E+01 3.00E-03 25.7
Fe 1.05E+01 1.3E+00 9.79E+00 7.3
K 2.33E+00 3.0E-01 2.26E+00 2.9
Li 1.60E+00 1.8E+00 1.49E+00 7.4
Mg 5.56E-01 1.0E+00 5.20E-01 6.9
Mn 1.55E+00 1.4E+00 1.46E+00 5.8
Na 8.85E+00 1.1E+00 8.52E+00 3.9
Ni 8.64E-01 1.2E+00 8.27E-01 4.4
Si NA NA 2.24E+01 NA
Ti 7.17E-01 1.5E+00 6.90E-01 3.8
Zr 1.04E-01 2.0E+00 9.60E-02 7.8
*All averages are based upon three replicate dissolutions and ICP-AES determinations NA = Not
applicable.
SRNL-STI-2011-00475, REVISION 0
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Table 3-7. Elemental concentrations of ARG standard from ICP-AES analysis of Aqua Regia, and Sodium
Peroxide/Hydroxide Fusion digestions performed concurrently with SB7b SRAT Product sample. Values are
presented on a weight percent (Wt%) total solids basis.
Aqua Regia*
Element Average %RSD Standard Value %Difference
(Measured vs
Standard Value)
Al 2.30E+00 1.2E+00 2.50E+00 -8.0
B 2.41E+00 2.9E-01 2.69E+00 -10.6
Ca 1.04E+00 6.8E-01 1.02E+00 1.5
Cr 6.68E-02 7.4E+00 6.40E-02 4.4
Cu 2.34E-03 7.0E+00 3.00E-03 -22.2
Fe 9.78E+00 1.2E+00 9.79E+00 -0.1
K 2.09E+00 1.7E+00 2.26E+00 -7.7
Li 1.50E+00 9.4E-01 1.49E+00 0.7
Mg 5.31E-01 7.5E+00 5.20E-01 2.1
9BMn 1.42E+00 1.0E+00 1.46E+00 -2.7
Na 8.48E+00 2.5E-01 8.52E+00 -0.5
Ni 8.26E-01 1.7E+00 8.27E-01 -0.1
Si 3.39E-01 1.4E+01 2.24E+01 -98.5
Ti 6.05E-01 7.2E+00 6.90E-01 -12.3
Zr 5.38E-02 1.7E+01 9.60E-02 -44.0
Sodium Peroxide/Hydroxide Fusion*
Element Average %RSD Known Value %Difference
(Measured vs
Known Value)
Al 2.58E+00 2.5E+00 2.50E+00 3.0
B 2.50E+00 2.0E+00 2.69E+00 -8.6
Ca 1.18E+00 1.2E+00 1.02E+00 15.7
Cr 7.29E-02 3.0E+00 6.40E-02 13.8
Cu <4.92E-03 NA 3.00E-03 NA
Fe 1.02E+01 2.1E+00 9.79E+00 3.7
K 2.30E+00 9.2E-01 2.26E+00 1.5
Li 1.51E+00 2.8E+00 1.49E+00 1.3
Mg 5.31E-01 9.3E-01 5.20E-01 2.0
Mn 1.51E+00 1.4E+00 1.46E+00 3.1
Na NA NA 8.52E+00 NA
Ni 8.36E-01 8.5E-01 8.27E-01 1.1
Si 2.36E+01 1.8E+00 2.24E+01 5.4
Ti 7.07E-01 1.8E+00 6.90E-01 2.5
Zr NA NA 9.60E-02 NA
*All averages are based upon two replicate dissolutions and ICP-AES determinations. NA = Not
applicable. <MDL = less than minimum detection limit.
SRNL-STI-2011-00475, REVISION 0
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Table 3-8. Continuation of elemental concentrations of ARG standard from ICP-AES analysis of Aqua Regia,
DWPF Cold Chem method and Sodium Peroxide/Hydroxide Fusion digestions performed concurrently with
SB7b SRAT Product sample. Values are presented on a weight percent (Wt%) total solids basis.
DWPF Cold Chem Method*
Element Average %RSD Known Value %Difference
(Measured vs
Known Value)
Al 2.45E+00 7.6E+00 2.50E+00 -2.0
B NA NA 2.69E+00 NA
Ca 1.07E+00 1.4E+01 1.02E+00 4.7
Cr 6.92E-02 4.6E+00 6.40E-02 8.1
Cu 3.93E-03 1.6E+01 3.00E-03 31.0
Fe 1.03E+01 6.1E+00 9.79E+00 5.1
K 2.29E+00 5.7E+00 2.26E+00 1.3
Li 1.54E+00 7.1E+00 1.49E+00 3.6
Mg 5.40E-01 1.0E+01 5.20E-01 3.8
Mn 1.52E+00 6.1E+00 1.46E+00 3.9
Na 8.98E+00 6.8E+00 8.52E+00 5.4
Ni 8.99E-01 5.9E+00 8.27E-01 8.7
Si NA NA 2.24E+01 NA
Ti 7.03E-01 6.2E+00 6.90E-01 1.8
Zr 1.01E-01 6.1E+00 9.60E-02 5.3
*All averages are based upon three replicate dissolutions and ICP-AES determinations NA = Not
applicable. <MDL = less than minimum detection limit.
Good recoveries were observed for most elements of significant weight percent in the ARG standards.
There are a few anomalies but based upon the %RSDs some of these elements were near the ICP-AES
detection limit. Upon review of the SRAT Receipt, SRAT Product and ARG data it is evident that not all
of the digestion issues seen with the radioactive sample are mirrored with the ARG standard. For
instance, the Al in the ARG appears to dissolve well in each digestion method as well as Fe. The SRAT
Receipt and SRAT Product have ~4 wt% more Fe than the ARG standard. The one and one-half hour
time frame allotted for the digestion may not be sufficient for dissolving all of the Fe and Mn in the initial
dilution of the samples. SB7b also contains some HM waste and some the different phases of aluminum
species present in the sludge slurry (boehmite and gibbsite among others) have less solubility in acid
matrices.
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4.0 3BCONCLUSIONS
The results from using the DWPF CC method to digest SB7b sludge slurry appear, in most cases, to be
equivalent to the AR and PF digestion methods. Visual observations indicate Fe and Mn may not be
completely dissolving in the initial dilution of the DWPF CC sample before the final dilution is
performed. However, ICP-AES analysis indicates the Fe and Mn mean concentration from all three
digestions are not statistically different. The DWPF should consider comparing the Fe and Mn results
obtained from PF digestion of the SRAT Product against the DWPF CC results and using the highest
average.
Aluminum (Al) and Th do not dissolve completely or are precipitated as fluoride salts. It is recommended
that these elements be determined from analysis of samples digested by the PF method.
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5.0 4BRECOMMENDATIONS
Based on the results from performing three different digestion methods on SB7b sludge slurry, SRNL
notes and recommends the following:
The results from using the DWPF CC method performed to digest SB7b sludge slurry appear, in
most cases, to be equivalent to the AR and PF digestion methods. However, Al, and Th should be
analyzed by the peroxide fusion method for SB7b. Visual observations indicate Fe and Mn may
not be completely dissolving in the initial dilution of the sample before the final dilution is
performed. However, for this data set, very small relative differences between the digestion
methods are noted and no statistical difference is observed between the digestion methods for Fe
and Mn. Fe and Mn concentration should be measured from both a CC and PF digestion of
SB7b sludge slurry and the highest concentration between the two digestions should be used.
Although K is a minor element, large relative differences are noted in this report between the
different digestions and the DWPF should also monitor the K concentration.
The DWPF CC method was originally developed to be used for SME analyses. Given continuous
visual observations of solids in the CC digestions both at SRNL and DWPF, potential issues with
accurate Al measurements when processing HM waste, and difficulty measuring Th accurately
due to the limited solubility of Th in HF matrices, SRNL recommends that the DWPF consider a
different digestion scheme that relieves some of these issues.
The DWPF CC results from this study indicate Al and Th do not completely dissolve or
precipitate as fluoride salts. Visual observations also indicate Fe and Mn may not
completely dissolve using the DWPF CC method. Therefore, DWPF should consider and
monitor the impact of these elements on SB7b blending operations conducted at DWPF
via comparison of SRAT and SME analyses. If a consistent difference in elemental
concentrations is revealed, another type of digestion (i.e. sodium peroxide/hydroxide fusion)
should be used to determine the concentration of the element in question. Particular emphasis
should be placed on monitoring Al, Fe, Mn, K, and Th concentrations in SB7b.
SRNL-STI-2011-00475, REVISION 0
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6.0 5BREFERENCES
1. C.J. Coleman, “Alkali Fusion Dissolutions of Sludge and Glass for Elemental and Anion
Analysis”, ADS Procedure ADS-2502, Rev. 6.
2. C.J. Coleman, “Aqua Regia Dissolution of Sludge for Elemental Analysis”, ADS
Procedure ADS-2226, Rev. 9.
3. JMP Statistical Discovery Software v 7.0.2; SAS Institute Inc., Cary, NC, 2008.
4. C.J. Coleman, F.M. Pennebaker, B.H. Burch and D.R. Click, “Evaluation of the DWPF
Cold Chem Dissolution Method with DWPF Sludge Batch 3 Simulant”, WSRC-TR-02-
00496, Rev. 0. See also D.R. Click, “Evaluation of the DWPF Cold Chem Dissolution
Method with Tank 7 and Tank 51 Radioactive Sludges”, WSRC-TR-2003-00580. D.R.
Click, C.J. Coleman, K.E. Zeigler and T.B. Edwards, “Sludge Batch Four (4) Defense
Waste Processing Facility (DWPF) Process Analytical Method Verification”, WSRC-
STI-2006-00025 Rev. 0. D. R. Click, T. B. Edwards, and M. A. Jones. “Verification of
the Defense Waste Processing Facility’s (DWPF) process digestion method for the
Sludge Batch 6 qualification sample”, WSRC-STI-2010-00259 Rev. 0. D.R. Click, T.B.
Edwards, M.A. Jones, and B.J. Wiedenman, “Verification of the Defense Waste
Processing Facility’s (DWPF) Process Digestion Method for the Sludge Batch 7a
Qualification Sample, SRNL-STI-2011-00158 Rev. 0.
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7.0 6BACKNOWLEDGEMENTS
The authors would like to acknowledge Monica Jenkins and Rita Sullivan.
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8.0 7BAPPENDIX A. SUPPORTING INFORMATION
SRNL-STI-2011-00475, REVISION 0
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Receipt Receipt Receipt Statistical Product Product Product Statistical
Element Aqua
Regia
Cold
Chem
Peroxide
Fusions Comparisons
Aqua
Regia
Cold
Chem
Peroxide
Fusions Comparisons
Al 8.478 8.140 8.830 CC < AR < PF 7.645 8.218 8.487 AR < CC < PF
B 0.008 . 0.081 AR < PF 0.008 . 0.017 AR < PF
Ca 0.638 0.662 0.753 AR < CC < PF 0.614 0.620 0.760 AR < CC < PF
Cr 0.043 0.044 0.060 AR < CC < PF 0.041 0.045 0.046 AR < CC < PF
Cu 0.080 0.044 0.049 CC < PF < AR 0.040 0.040 0.044 CC < AR < PF
Fe 14.225 14.475 14.300 AR < PF < CC 13.740 13.750 13.644 PF < AR < CC
K 0.026 0.188 0.255 AR < CC < PF 0.055 0.128 0.289 AR < CC < PF
Li 0.026 0.025 0.023 PF < CC < AR 0.025 0.026 0.025 PF < AR < CC
Mg 0.285 0.296 0.277 PF < AR < CC 0.278 0.293 0.274 PF < AR < CC
Mn 3.015 3.123 2.980 PF < AR < CC 2.935 3.015 2.974 AR < PF < CC
Na 14.125 14.575 . AR < CC 14.894 15.125 . AR < CC
Ni 2.935 2.975 2.953 AR < PF < CC 2.815 2.823 2.757 PF < AR < CC
Si 0.472 . 1.057 AR < PF 0.420 . 1.070 AR < PF
Th 1.036 0.761 0.956 CC < PF < AR 1.063 0.727 0.940 CC < PF < AR
Ti 0.017 0.019 0.020 AR < CC <PF 0.020 0.015 0.020 CC < PF < AR
U 4.773 4.980 4.453 PF < AR < CC 4.480 4.510 4.260 PF < AR < CC
Zr 0.139 0.270 . AR < CC 0.150 0.254 . AR < CC
SRNL-STI-2011-00475, REVISION 0
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Variability Chart for Al
Al
7.5
8.0
8.5
9.0
Avg=8.266818
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
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02
88
12
1
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12
3
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88
12
4
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02
88
12
6
30
02
88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
90
1
30
02
86
90
2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
11
5
30
02
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7
30
02
86
88
4
30
02
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88
5
30
02
86
88
6
LIMS #
Aq
ua R
eg
ia
Co
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Pero
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Fu
sio
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Aq
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Co
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Pero
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ns Prep
Product Receipt Type
SB7b SRAT Grouping
Variability Chart for B
B
0.00
0.01
0.02
0.03
0.04
0.05
0.06
0.07
0.08
0.09
Avg=0.025531
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
30
02
88
12
1
30
02
88
12
3
30
02
88
12
4
30
02
88
12
6
30
02
88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
90
1
30
02
86
90
2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
11
5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
Aq
ua R
eg
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Co
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Aq
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eg
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Co
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hem
Pero
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sio
ns Prep
Product Receipt Type
SB7b SRAT Grouping
Variability Chart for Ca
Ca
0.60
0.65
0.70
0.75
0.80
Avg=0.666818
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
30
02
88
12
1
30
02
88
12
3
30
02
88
12
4
30
02
88
12
6
30
02
88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
90
1
30
02
86
90
2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
11
5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
Aq
ua R
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Co
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Pero
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Aq
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Co
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Pero
xid
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Fu
sio
ns Prep
Product Receipt Type
SB7b SRAT Grouping
Variability Chart for Cr
Cr
0.040
0.045
0.050
0.055
0.060
0.065
0.070
0.075
Avg=0.045977
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
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1
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3
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88
12
6
30
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88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
90
1
30
02
86
90
2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
11
5
30
02
88
11
7
30
02
86
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4
30
02
86
88
5
30
02
86
88
6
LIMS #
Aq
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Aq
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Co
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hem
Pero
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sio
ns Prep
Product Receipt Type
SB7b SRAT Grouping
SRNL-STI-2011-00475, REVISION 0
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Variability Chart for Cu
Cu
0.04
0.05
0.06
0.07
0.08
Avg=0.049809
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
30
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1
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3
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4
30
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88
12
6
30
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88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
90
1
30
02
86
90
2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
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5
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7
30
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4
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88
5
30
02
86
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6
LIMS #
Aq
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Aq
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Co
ld C
hem
Pero
xid
e
Fu
sio
ns Prep
Product Receipt Type
SB7b SRAT Grouping
Variability Chart for Fe
Fe
13.0
13.5
14.0
14.5
15.0
Avg=14.02682
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
30
02
88
12
1
30
02
88
12
3
30
02
88
12
4
30
02
88
12
6
30
02
88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
90
1
30
02
86
90
2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
11
5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
Aq
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Pero
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ns
Aq
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Co
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hem
Pero
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Fu
sio
ns Prep
Product Receipt Type
SB7b SRAT Grouping
Variability Chart for K
K
0.00
0.05
0.10
0.15
0.20
0.25
0.30
0.35
Avg=0.146518
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
30
02
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12
1
30
02
88
12
3
30
02
88
12
4
30
02
88
12
6
30
02
88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
90
1
30
02
86
90
2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
11
5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
Aq
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Pero
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Aq
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Co
ld C
hem
Pero
xid
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Fu
sio
ns Prep
Product Receipt Type
SB7b SRAT Grouping
Variability Chart for Li
Li
0.023
0.024
0.025
0.026
0.027
0.028
Avg=0.025359
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
30
02
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12
1
30
02
88
12
3
30
02
88
12
4
30
02
88
12
6
30
02
88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
90
1
30
02
86
90
2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
11
5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
Aq
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Co
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Pero
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ns
Aq
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Co
ld C
hem
Pero
xid
e
Fu
sio
ns Prep
Product Receipt Type
SB7b SRAT Grouping
SRNL-STI-2011-00475, REVISION 0
41
Variability Chart for Mg
Mg
0.26
0.27
0.28
0.29
0.30
0.31
Avg=0.284545
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
30
02
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1
30
02
88
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3
30
02
88
12
4
30
02
88
12
6
30
02
88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
90
1
30
02
86
90
2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
11
5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
Aq
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Pero
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Aq
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Co
ld C
hem
Pero
xid
e
Fu
sio
ns Prep
Product Receipt Type
SB7b SRAT Grouping
Variability Chart for Mn
Mn
2.80
2.85
2.90
2.95
3.00
3.05
3.10
3.15
3.20
Avg=3.009682
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
30
02
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12
1
30
02
88
12
3
30
02
88
12
4
30
02
88
12
6
30
02
88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
90
1
30
02
86
90
2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
11
5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
Aq
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Aq
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Co
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hem
Pero
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Fu
sio
ns Prep
Product Receipt Type
SB7b SRAT Grouping
Variability Chart for Na
Na
13.5
14.0
14.5
15.0
15.5
Avg=14.67975
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
30
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1
30
02
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12
3
30
02
88
12
4
30
02
88
12
6
30
02
88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
90
1
30
02
86
90
2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
11
5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
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Aq
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Co
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hem
Pero
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Fu
sio
ns Prep
Product Receipt Type
SB7b SRAT Grouping
Variability Chart for Ni
Ni
2.6
2.7
2.8
2.9
3.0
3.1
Avg=2.878091
30
02
88
46
2
30
02
88
46
3
30
02
88
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4
30
02
88
46
5
30
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1
30
02
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3
30
02
88
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4
30
02
88
12
6
30
02
88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
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90
1
30
02
86
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2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
11
5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
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Aq
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hem
Pero
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Fu
sio
ns Prep
Product Receipt Type
SB7b SRAT Grouping
SRNL-STI-2011-00475, REVISION 0
42
Variability Chart for Si
Si
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0
1.1
Avg=0.7105
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
30
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1
30
02
88
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3
30
02
88
12
4
30
02
88
12
6
30
02
88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
90
1
30
02
86
90
2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
11
5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
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Aq
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Co
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hem
Pero
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Fu
sio
ns Prep
Product Receipt Type
SB7b SRAT Grouping
Variability Chart for Th
Th
0.6
0.7
0.8
0.9
1.0
1.1
Avg=0.910682
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
30
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1
30
02
88
12
3
30
02
88
12
4
30
02
88
12
6
30
02
88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
90
1
30
02
86
90
2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
88
11
5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
Aq
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Aq
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Pero
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ns Prep
Product Receipt Type
SB7b SRAT Grouping
Variability Chart for Ti
Ti
0.014
0.015
0.016
0.017
0.018
0.019
0.020
0.021
0.022
Avg=0.018323
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
30
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88
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1
30
02
88
12
3
30
02
88
12
4
30
02
88
12
6
30
02
88
60
0
30
02
88
60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
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1
30
02
86
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2
30
02
86
90
3
30
02
88
11
2
30
02
88
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4
30
02
88
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5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
Aq
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Aq
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Co
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Pero
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ns Prep
Product Receipt Type
SB7b SRAT Grouping
Variability Chart for U
U
4.1
4.2
4.3
4.4
4.5
4.6
4.7
4.8
4.9
5.0
Avg=4.595909
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
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5
30
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1
30
02
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3
30
02
88
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4
30
02
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6
30
02
88
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0
30
02
88
60
1
30
02
88
60
3
30
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86
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0
30
02
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1
30
02
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2
30
02
86
90
3
30
02
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11
2
30
02
88
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4
30
02
88
11
5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
Aq
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Aq
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Co
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Pero
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Fu
sio
ns Prep
Product Receipt Type
SB7b SRAT Grouping
SRNL-STI-2011-00475, REVISION 0
43
Variability Chart for Zr
Zr
0.10
0.15
0.20
0.25
Avg=0.203063
30
02
88
46
2
30
02
88
46
3
30
02
88
46
4
30
02
88
46
5
30
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1
30
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3
30
02
88
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4
30
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6
30
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0
30
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60
1
30
02
88
60
3
30
02
86
90
0
30
02
86
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1
30
02
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2
30
02
86
90
3
30
02
88
11
2
30
02
88
11
4
30
02
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11
5
30
02
88
11
7
30
02
86
88
4
30
02
86
88
5
30
02
86
88
6
LIMS #
Aq
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Aq
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Pero
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ns Prep
Product Receipt Type
SB7b SRAT Grouping
SRNL-STI-2011-00475, REVISION 0
44
Oneway Analysis of Al By Prep Grouping=SB7b SRAT, Type=Product
7.25
7.5
7.75
8
8.25
8.5
8.75
Al
Aq
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Co
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Pero
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ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.61932
Adj Rsquare 0.52415
Root Mean Square Error 0.3195
Mean of Response 8.082727
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 1.3285765 0.664288 6.5075 0.0210
Error 8 0.8166417 0.102080
C. Total 10 2.1452182
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 7.64500 0.15975 7.2766 8.0134
Cold Chem 4 8.21750 0.15975 7.8491 8.5859
Peroxide Fusions 3 8.48667 0.18446 8.0613 8.9120
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 7.64500 0.220681 0.11034 7.2938 7.9962
Cold Chem 4 8.21750 0.464785 0.23239 7.4779 8.9571
Peroxide Fusions 3 8.48667 0.105987 0.06119 8.2234 8.7500
Tests that the Variances are Equal
0.0
0.1
0.2
0.3
0.4
0.5
Std
Dev
Aq
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Pero
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Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.2206808 0.1700000 0.1700000
Cold Chem 4 0.4647849 0.3925000 0.3925000
Peroxide Fusions 3 0.1059874 0.0755556 0.0966667
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 5.4182 2 8 0.0325
Brown-Forsythe 10.3737 2 8 0.0060
Levene 11.3059 2 8 0.0047
Bartlett 1.8682 2 . 0.1544
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
19.6462 2 4.9463 0.0044
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Peroxide Fusions A 8.4866667
Cold Chem A B 8.2175000
Aqua Regia B 7.6450000
Levels not connected by same letter are significantly different.
Oneway Analysis of B By Prep Grouping=SB7b SRAT, Type=Product
0.007
0.009
0.011
0.013
0.015
0.017
B
Aq
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Prep
Missing Rows 4
Oneway Anova
Summary of Fit
Rsquare 0.99663
Adj Rsquare 0.995956
Root Mean Square Error 0.000313
Mean of Response 0.011818
Observations (or Sum Wgts) 7
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 1 0.00014514 0.000145 1478.793 <.0001
Error 5 0.00000049 9.815e-8
C. Total 6 0.00014563
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.007875 0.00016 0.00747 0.00828
Cold Chem 0 . . . .
Peroxide Fusions 3 0.017076 0.00018 0.01661 0.01754
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.007875 0.000096 4.79e-5 0.00772 0.00803
Cold Chem 0 . . . . .
Peroxide Fusions 3 0.017076 0.000481 0.00028 0.01588 0.01827
Tests that the Variances are Equal
0
0.0001
0.0002
0.0003
0.0004
0.0005
Std
Dev
Aq
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Co
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hem
Pero
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Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0000957 0.0000750 0.0000750
Cold Chem 0 . 0.0000000 0.0000000
Peroxide Fusions 3 0.0004813 0.0003672 0.0003390
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 2.3384 1 5 0.1868
Brown-Forsythe 2.1578 1 5 0.2018
Levene 11.5000 1 5 0.0194
Bartlett 4.4549 1 . 0.0348
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
1064.9960 1 2.1192 0.0007
SRNL-STI-2011-00475, REVISION 0
45
Oneway Analysis of Ca By Prep Grouping=SB7b SRAT, Type=Product
0.6
0.65
0.7
0.75
0.8
Ca
Aq
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Co
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hem
Pero
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Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.858524
Adj Rsquare 0.823155
Root Mean Square Error 0.030422
Mean of Response 0.655727
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.04492843 0.022464 24.2733 0.0004
Error 8 0.00740375 0.000925
C. Total 10 0.05233218
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.613500 0.01521 0.57842 0.64858
Cold Chem 4 0.619750 0.01521 0.58467 0.65483
Peroxide Fusions 3 0.760000 0.01756 0.71950 0.80050
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.613500 0.024420 0.01221 0.57464 0.65236
Cold Chem 4 0.619750 0.028477 0.01424 0.57444 0.66506
Peroxide Fusions 3 0.760000 0.039887 0.02303 0.66091 0.85909
Tests that the Variances are Equal
0.000
0.010
0.020
0.030
0.040
Std
Dev
Aq
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Co
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hem
Pero
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Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0244199 0.0162500 0.0160000
Cold Chem 4 0.0284766 0.0232500 0.0232500
Peroxide Fusions 3 0.0398873 0.0300000 0.0310000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 0.5822 2 8 0.5807
Brown-Forsythe 0.6804 2 8 0.5335
Levene 0.8813 2 8 0.4509
Bartlett 0.2689 2 . 0.7642
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
14.6815 2 4.5232 0.0105
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Peroxide Fusions A 0.76000000
Cold Chem B 0.61975000
Aqua Regia B 0.61350000
Levels not connected by same letter are significantly different.
Oneway Analysis of Cr By Prep Grouping=SB7b SRAT, Type=Product
0.038
0.04
0.042
0.044
0.046
0.048
0.05
Cr
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.524084
Adj Rsquare 0.405104
Root Mean Square Error 0.002298
Mean of Response 0.043691
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.00004652 0.000023 4.4048 0.0513
Error 8 0.00004225 5.281e-6
C. Total 10 0.00008877
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.041000 0.00115 0.03835 0.04365
Cold Chem 4 0.044900 0.00115 0.04225 0.04755
Peroxide Fusions 3 0.045667 0.00133 0.04261 0.04873
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.041000 0.001633 0.00082 0.03840 0.04360
Cold Chem 4 0.044900 0.003140 0.00157 0.03990 0.04990
Peroxide Fusions 3 0.045667 0.001528 0.00088 0.04187 0.04946
Tests that the Variances are Equal
0
0.001
0.002
0.003
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0016330 0.0010000 0.0010000
Cold Chem 4 0.0031401 0.0022500 0.0021500
Peroxide Fusions 3 0.0015275 0.0011111 0.0013333
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 0.7659 2 8 0.4962
Brown-Forsythe 0.5384 2 8 0.6034
Levene 1.0358 2 8 0.3981
Bartlett 0.7712 2 . 0.4625
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
7.1397 2 5.0708 0.0335
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Peroxide Fusions A 0.04566667
Cold Chem A 0.04490000
Aqua Regia A 0.04100000
Levels not connected by same letter are significantly different.
SRNL-STI-2011-00475, REVISION 0
46
Oneway Analysis of Cu By Prep Grouping=SB7b SRAT, Type=Product
0.037
0.038
0.039
0.04
0.041
0.042
0.043
0.044
0.045
Cu
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.598679
Adj Rsquare 0.498349
Root Mean Square Error 0.001512
Mean of Response 0.0411
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.00002728 0.000014 5.9671 0.0259
Error 8 0.00001828 2.286e-6
C. Total 10 0.00004556
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.040250 0.00076 0.03851 0.04199
Cold Chem 4 0.040025 0.00076 0.03828 0.04177
Peroxide Fusions 3 0.043667 0.00087 0.04165 0.04568
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.040250 0.001708 0.00085 0.03753 0.04297
Cold Chem 4 0.040025 0.001719 0.00086 0.03729 0.04276
Peroxide Fusions 3 0.043667 0.000577 0.00033 0.04223 0.04510
Tests that the Variances are Equal
0
0.0005
0.001
0.0015
0.002
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0017078 0.0012500 0.0012500
Cold Chem 4 0.0017193 0.0013750 0.0013750
Peroxide Fusions 3 0.0005774 0.0004444 0.0003333
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 0.8060 2 8 0.4798
Brown-Forsythe 1.7246 2 8 0.2384
Levene 1.7275 2 8 0.2379
Bartlett 1.0000 2 . 0.3679
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
11.4664 2 4.8685 0.0144
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Peroxide Fusions A 0.04366667
Aqua Regia B 0.04025000
Cold Chem B 0.04002500
Levels not connected by same letter are significantly different.
Oneway Analysis of Fe By Prep Grouping=SB7b SRAT, Type=Product
13
13.5
14
14.5
Fe
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.009525
Adj Rsquare -0.23809
Root Mean Square Error 0.539209
Mean of Response 13.71727
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.0223672 0.011184 0.0385 0.9624
Error 8 2.3259670 0.290746
C. Total 10 2.3483342
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 13.7395 0.26960 13.118 14.361
Cold Chem 4 13.7500 0.26960 13.128 14.372
Peroxide Fusions 3 13.6440 0.31131 12.926 14.362
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 13.7395 0.479878 0.23994 12.976 14.503
Cold Chem 4 13.7500 0.732575 0.36629 12.584 14.916
Peroxide Fusions 3 13.6440 0.112067 0.06470 13.366 13.922
Tests that the Variances are Equal
0.0
0.2
0.4
0.6
0.8
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.4798781 0.3920000 0.3920000
Cold Chem 4 0.7325754 0.6000000 0.6000000
Peroxide Fusions 3 0.1120669 0.0846667 0.0850000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 2.3848 2 8 0.1540
Brown-Forsythe 6.3057 2 8 0.0227
Levene 7.2966 2 8 0.0157
Bartlett 2.1918 2 . 0.1117
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
0.0952 2 4.3712 0.9110
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Cold Chem A 13.750000
Aqua Regia A 13.739500
Peroxide Fusions A 13.644000
Levels not connected by same letter are significantly different.
SRNL-STI-2011-00475, REVISION 0
47
Oneway Analysis of K By Prep Grouping=SB7b SRAT, Type=Product
0.05
0.1
0.15
0.2
0.25
0.3
0.35
K
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.970568
Adj Rsquare 0.96321
Root Mean Square Error 0.01906
Mean of Response 0.145636
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.09583438 0.047917 131.9049 <.0001
Error 8 0.00290617 0.000363
C. Total 10 0.09874055
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.055250 0.00953 0.03327 0.07723
Cold Chem 4 0.128250 0.00953 0.10627 0.15023
Peroxide Fusions 3 0.289333 0.01100 0.26396 0.31471
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.055250 0.002500 0.00125 0.05127 0.05923
Cold Chem 4 0.128250 0.000957 0.00048 0.12673 0.12977
Peroxide Fusions 3 0.289333 0.037978 0.02193 0.19499 0.38368
Tests that the Variances are Equal
0.000
0.010
0.020
0.030
0.040
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0025000 0.0017500 0.0017500
Cold Chem 4 0.0009574 0.0007500 0.0007500
Peroxide Fusions 3 0.0379781 0.0291111 0.0253333
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 2.5730 2 8 0.1371
Brown-Forsythe 2.5047 2 8 0.1430
Levene 19.4175 2 8 0.0009
Bartlett 11.6633 2 . <.0001
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
1275.4589 2 3.5152 <.0001
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Peroxide Fusions A 0.28933333
Cold Chem B 0.12825000
Aqua Regia C 0.05525000
Levels not connected by same letter are significantly different.
Oneway Analysis of Li By Prep Grouping=SB7b SRAT, Type=Product
0.024
0.025
0.026
0.027
0.028
Li
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.197216
Adj Rsquare -0.00348
Root Mean Square Error 0.001506
Mean of Response 0.025618
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.00000446 2.2282e-6 0.9827 0.4153
Error 8 0.00001814 2.2675e-6
C. Total 10 0.00002260
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.025250 0.00075 0.02351 0.02699
Cold Chem 4 0.026450 0.00075 0.02471 0.02819
Peroxide Fusions 3 0.025000 0.00087 0.02300 0.02700
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.025250 0.001258 0.00063 0.02325 0.02725
Cold Chem 4 0.026450 0.001949 0.00097 0.02335 0.02955
Peroxide Fusions 3 0.025000 0.001000 0.00058 0.02252 0.02748
Tests that the Variances are Equal
0
0.0005
0.001
0.0015
0.002
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0012583 0.0008750 0.0007500
Cold Chem 4 0.0019485 0.0016500 0.0016500
Peroxide Fusions 3 0.0010000 0.0006667 0.0010000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 1.7959 2 8 0.2269
Brown-Forsythe 2.0948 2 8 0.1855
Levene 2.7691 2 8 0.1219
Bartlett 0.4978 2 . 0.6079
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
0.7382 2 5.2324 0.5219
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Cold Chem A 0.02645000
Aqua Regia A 0.02525000
Peroxide Fusions A 0.02500000
Levels not connected by same letter are significantly different.
SRNL-STI-2011-00475, REVISION 0
48
Oneway Analysis of Mg By Prep Grouping=SB7b SRAT, Type=Product
0.26
0.27
0.28
0.29
0.3
0.31
Mg
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.41157
Adj Rsquare 0.264463
Root Mean Square Error 0.011125
Mean of Response 0.282455
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.00069256 0.000346 2.7978 0.1199
Error 8 0.00099017 0.000124
C. Total 10 0.00168273
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.278250 0.00556 0.26542 0.29108
Cold Chem 4 0.292750 0.00556 0.27992 0.30558
Peroxide Fusions 3 0.274333 0.00642 0.25952 0.28915
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.278250 0.010720 0.00536 0.26119 0.29531
Cold Chem 4 0.292750 0.014431 0.00722 0.26979 0.31571
Peroxide Fusions 3 0.274333 0.003215 0.00186 0.26635 0.28232
Tests that the Variances are Equal
0.000
0.005
0.010
0.015
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0107199 0.0071250 0.0067500
Cold Chem 4 0.0144309 0.0117500 0.0117500
Peroxide Fusions 3 0.0032146 0.0024444 0.0023333
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 1.3460 2 8 0.3134
Brown-Forsythe 2.1885 2 8 0.1745
Levene 2.7563 2 8 0.1229
Bartlett 1.5456 2 . 0.2132
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
2.7742 2 4.607 0.1619
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Cold Chem A 0.29275000
Aqua Regia A 0.27825000
Peroxide Fusions A 0.27433333
Levels not connected by same letter are significantly different.
Oneway Analysis of Mn By Prep Grouping=SB7b SRAT, Type=Product
2.8
2.85
2.9
2.95
3
3.05
3.1
3.15
3.2
Mn
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.106136
Adj Rsquare -0.11733
Root Mean Square Error 0.116087
Mean of Response 2.974818
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.01280097 0.006400 0.4750 0.6384
Error 8 0.10780867 0.013476
C. Total 10 0.12060964
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 2.93500 0.05804 2.8012 3.0688
Cold Chem 4 3.01500 0.05804 2.8812 3.1488
Peroxide Fusions 3 2.97433 0.06702 2.8198 3.1289
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 2.93500 0.105780 0.05289 2.7667 3.1033
Cold Chem 4 3.01500 0.155456 0.07773 2.7676 3.2624
Peroxide Fusions 3 2.97433 0.029501 0.01703 2.9010 3.0476
Tests that the Variances are Equal
0.00
0.05
0.10
0.15
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.1057796 0.0880000 0.0880000
Cold Chem 4 0.1554563 0.1250000 0.1250000
Peroxide Fusions 3 0.0295014 0.0224444 0.0213333
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 1.8779 2 8 0.2145
Brown-Forsythe 4.0354 2 8 0.0614
Levene 5.6634 2 8 0.0294
Bartlett 1.8257 2 . 0.1611
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
0.3543 2 4.5137 0.7196
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Cold Chem A 3.0150000
Peroxide Fusions A 2.9743333
Aqua Regia A 2.9350000
Levels not connected by same letter are significantly different.
SRNL-STI-2011-00475, REVISION 0
49
Oneway Analysis of Na By Prep Grouping=SB7b SRAT, Type=Product
14
14.5
15
15.5
Na
Aq
ua R
eg
ia
Co
ld C
hem
Prep
Missing Rows 3
Oneway Anova
Summary of Fit
Rsquare 0.041245
Adj Rsquare -0.11855
Root Mean Square Error 0.643016
Mean of Response 15.0095
Observations (or Sum Wgts) 8
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 1 0.1067220 0.106722 0.2581 0.6296
Error 6 2.4808140 0.413469
C. Total 7 2.5875360
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 14.8940 0.32151 14.107 15.681
Cold Chem 4 15.1250 0.32151 14.338 15.912
Peroxide Fusions 0 . . . .
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 14.8940 0.551759 0.27588 14.016 15.772
Cold Chem 4 15.1250 0.722842 0.36142 13.975 16.275
Peroxide Fusions 0 . . . . .
Tests that the Variances are Equal
0.0
0.2
0.4
0.6
0.8
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.5517590 0.4660000 0.4660000
Cold Chem 4 0.7228416 0.5750000 0.5750000
Peroxide Fusions 0 . 0.0000000 0.0000000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 0.5430 1 6 0.4890
Brown-Forsythe 0.3329 1 6 0.5850
Levene 0.4922 1 6 0.5093
Bartlett 0.1853 1 . 0.6668
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
0.2581 1 5.6099 0.6308
Oneway Analysis of Ni By Prep Grouping=SB7b SRAT, Type=Product
2.6
2.65
2.7
2.75
2.8
2.85
2.9
2.95
3
Ni
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.081113
Adj Rsquare -0.14861
Root Mean Square Error 0.109516
Mean of Response 2.801636
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.00846988 0.004235 0.3531 0.7129
Error 8 0.09595067 0.011994
C. Total 10 0.10442055
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 2.81450 0.05476 2.6882 2.9408
Cold Chem 4 2.82250 0.05476 2.6962 2.9488
Peroxide Fusions 3 2.75667 0.06323 2.6109 2.9025
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 2.81450 0.100348 0.05017 2.6548 2.9742
Cold Chem 4 2.82250 0.145917 0.07296 2.5903 3.0547
Peroxide Fusions 3 2.75667 0.030551 0.01764 2.6808 2.8326
Tests that the Variances are Equal
0.00
0.05
0.10
0.15
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.1003477 0.0835000 0.0835000
Cold Chem 4 0.1459166 0.1175000 0.1175000
Peroxide Fusions 3 0.0305505 0.0222222 0.0266667
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 1.8618 2 8 0.2168
Brown-Forsythe 3.7174 2 8 0.0722
Levene 5.5238 2 8 0.0311
Bartlett 1.6656 2 . 0.1891
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
0.7921 2 4.5952 0.5063
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Cold Chem A 2.8225000
Aqua Regia A 2.8145000
Peroxide Fusions A 2.7566667
Levels not connected by same letter are significantly different.
SRNL-STI-2011-00475, REVISION 0
50
Oneway Analysis of Si By Prep Grouping=SB7b SRAT, Type=Product
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1
1.1
Si
Aq
ua R
eg
ia
Pero
xid
e
Fu
sio
ns
Prep
Missing Rows 4
Oneway Anova
Summary of Fit
Rsquare 0.973129
Adj Rsquare 0.967754
Root Mean Square Error 0.063246
Mean of Response 0.698571
Observations (or Sum Wgts) 7
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 1 0.72428571 0.724286 181.0714 <.0001
Error 5 0.02000000 0.004000
C. Total 6 0.74428571
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.42000 0.03162 0.33871 0.5013
Cold Chem 0 . . . .
Peroxide Fusions 3 1.07000 0.03651 0.97614 1.1639
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.42000 0.081240 0.04062 0.2907 0.5493
Cold Chem 0 . . . . .
Peroxide Fusions 3 1.07000 0.010000 0.00577 1.0452 1.0948
Tests that the Variances are Equal
0.00
0.02
0.04
0.06
0.08
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0812404 0.0600000 0.0450000
Cold Chem 0 . 0.0000000 0.0000000
Peroxide Fusions 3 0.0100000 0.0066667 0.0100000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 1.0519 1 5 0.3521
Brown-Forsythe 0.6863 1 5 0.4452
Levene 4.4599 1 5 0.0884
Bartlett 4.8513 1 . 0.0276
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
250.9901 1 3.1205 0.0004
Oneway Analysis of Th By Prep Grouping=SB7b SRAT, Type=Product
0.6
0.7
0.8
0.9
1
1.1
Th
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.855208
Adj Rsquare 0.81901
Root Mean Square Error 0.069651
Mean of Response 0.907182
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.22922789 0.114614 23.6258 0.0004
Error 8 0.03880975 0.004851
C. Total 10 0.26803764
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 1.06250 0.03483 0.98219 1.1428
Cold Chem 4 0.72725 0.03483 0.64694 0.8076
Peroxide Fusions 3 0.94000 0.04021 0.84727 1.0327
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 1.06250 0.039476 0.01974 0.99969 1.1253
Cold Chem 4 0.72725 0.096497 0.04825 0.57370 0.8808
Peroxide Fusions 3 0.94000 0.055678 0.03215 0.80169 1.0783
Tests that the Variances are Equal
0.00
0.02
0.04
0.06
0.08
0.10
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
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Fu
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ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0394757 0.0325000 0.0325000
Cold Chem 4 0.0964965 0.0792500 0.0792500
Peroxide Fusions 3 0.0556776 0.0400000 0.0500000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 2.2531 2 8 0.1674
Brown-Forsythe 4.2922 2 8 0.0541
Levene 4.2217 2 8 0.0560
Bartlett 0.9997 2 . 0.3680
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
19.7785 2 4.5038 0.0059
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Aqua Regia A 1.0625000
Peroxide Fusions A 0.9400000
Cold Chem B 0.7272500
Levels not connected by same letter are significantly different.
SRNL-STI-2011-00475, REVISION 0
51
Oneway Analysis of Ti By Prep Grouping=SB7b SRAT, Type=Product
0.014
0.015
0.016
0.017
0.018
0.019
0.02
0.021
Ti
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.993964
Adj Rsquare 0.992455
Root Mean Square Error 0.000226
Mean of Response 0.018127
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.00006751 0.000034 658.6519 <.0001
Error 8 0.00000041 5.125e-8
C. Total 10 0.00006792
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.020000 0.00011 0.01974 0.02026
Cold Chem 4 0.014850 0.00011 0.01459 0.01511
Peroxide Fusions 3 0.020000 0.00013 0.01970 0.02030
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.020000 0.000000 0.00000 0.02000 0.02000
Cold Chem 4 0.014850 0.000370 0.00018 0.01426 0.01544
Peroxide Fusions 3 0.020000 0.000000 0.00000 0.02000 0.02000
Tests that the Variances are Equal
0
0.0001
0.0002
0.0003
0.0004
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
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Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0000000 0.0000000 0.0000000
Cold Chem 4 0.0003697 0.0003000 0.0003000
Peroxide Fusions 3 0.0000000 0.0000000 0.0000000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 3.7208 2 8 0.0720
Brown-Forsythe 15.2727 2 8 0.0019
Levene 18.3273 2 8 0.0010
Bartlett . 2 . .
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
. 2 . .
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Aqua Regia A 0.02000000
Peroxide Fusions A 0.02000000
Cold Chem B 0.01485000
Levels not connected by same letter are significantly different.
Oneway Analysis of U By Prep Grouping=SB7b SRAT, Type=Product
4.2
4.3
4.4
4.5
4.6
4.7
U
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.361496
Adj Rsquare 0.20187
Root Mean Square Error 0.164317
Mean of Response 4.430909
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.12229091 0.061145 2.2646 0.1662
Error 8 0.21600000 0.027000
C. Total 10 0.33829091
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 4.48000 0.08216 4.2905 4.6695
Cold Chem 4 4.51000 0.08216 4.3205 4.6995
Peroxide Fusions 3 4.26000 0.09487 4.0412 4.4788
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 4.48000 0.165731 0.08287 4.2163 4.7437
Cold Chem 4 4.51000 0.182392 0.09120 4.2198 4.8002
Peroxide Fusions 3 4.26000 0.130000 0.07506 3.9371 4.5829
Tests that the Variances are Equal
0.00
0.05
0.10
0.15
0.20
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
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Fu
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ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.1657307 0.1400000 0.1400000
Cold Chem 4 0.1823915 0.1350000 0.1350000
Peroxide Fusions 3 0.1300000 0.1000000 0.0800000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 0.2388 2 8 0.7930
Brown-Forsythe 0.4110 2 8 0.6763
Levene 0.3594 2 8 0.7088
Bartlett 0.1105 2 . 0.8953
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
2.6031 2 5.258 0.1638
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Cold Chem A 4.5100000
Aqua Regia A 4.4800000
Peroxide Fusions A 4.2600000
Levels not connected by same letter are significantly different.
SRNL-STI-2011-00475, REVISION 0
52
Oneway Analysis of Zr By Prep Grouping=SB7b SRAT, Type=Product
0.125
0.15
0.175
0.2
0.225
0.25
0.275
Zr
Aq
ua R
eg
ia
Co
ld C
hem
Prep
Missing Rows 3
Oneway Anova
Summary of Fit
Rsquare 0.933712
Adj Rsquare 0.922665
Root Mean Square Error 0.015922
Mean of Response 0.20175
Observations (or Sum Wgts) 8
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 1 0.02142450 0.021424 84.5148 <.0001
Error 6 0.00152100 0.000254
C. Total 7 0.02294550
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.150000 0.00796 0.13052 0.16948
Cold Chem 4 0.253500 0.00796 0.23402 0.27298
Peroxide Fusions 0 . . . .
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.150000 0.016330 0.00816 0.12402 0.17598
Cold Chem 4 0.253500 0.015503 0.00775 0.22883 0.27817
Peroxide Fusions 0 . . . . .
Tests that the Variances are Equal
0.000
0.005
0.010
0.015
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
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Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0163299 0.0100000 0.0100000
Cold Chem 4 0.0155027 0.0130000 0.0130000
Peroxide Fusions 0 . 0.0000000 0.0000000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 0.0157 1 6 0.9044
Brown-Forsythe 0.2379 1 6 0.6430
Levene 0.2427 1 6 0.6398
Bartlett 0.0069 1 . 0.9336
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
84.5148 1 5.9839 <.0001
Oneway Analysis of Al By Prep Grouping=SB7b SRAT, Type=Receipt
7.8
8
8.2
8.4
8.6
8.8
Al
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.645092
Adj Rsquare 0.556365
Root Mean Square Error 0.237559
Mean of Response 8.450909
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.8206159 0.410308 7.2705 0.0159
Error 8 0.4514750 0.056434
C. Total 10 1.2720909
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 8.47750 0.11878 8.2036 8.7514
Cold Chem 4 8.14000 0.11878 7.8661 8.4139
Peroxide Fusions 3 8.83000 0.13715 8.5137 9.1463
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 8.47750 0.323767 0.16188 7.9623 8.9927
Cold Chem 4 8.14000 0.212603 0.10630 7.8017 8.4783
Peroxide Fusions 3 8.83000 0.026458 0.01528 8.7643 8.8957
Tests that the Variances are Equal
0.00
0.10
0.20
0.30
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
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Fu
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ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.3237669 0.2725000 0.2725000
Cold Chem 4 0.2126029 0.1700000 0.1700000
Peroxide Fusions 3 0.0264575 0.0200000 0.0200000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 3.6496 2 8 0.0748
Brown-Forsythe 10.2523 2 8 0.0062
Levene 11.6207 2 8 0.0043
Bartlett 3.2327 2 . 0.0395
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
19.6278 2 4.1146 0.0079
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Peroxide Fusions A 8.8300000
Aqua Regia A B 8.4775000
Cold Chem B 8.1400000
Levels not connected by same letter are significantly different.
SRNL-STI-2011-00475, REVISION 0
53
Oneway Analysis of B By Prep Grouping=SB7b SRAT, Type=Receipt
0
0.01
0.02
0.03
0.04
0.05
0.06
0.07
0.08
0.09
B
Aq
ua R
eg
ia
Pero
xid
e
Fu
sio
ns
Prep
Missing Rows 4
Oneway Anova
Summary of Fit
Rsquare 0.999962
Adj Rsquare 0.999955
Root Mean Square Error 0.000262
Mean of Response 0.039244
Observations (or Sum Wgts) 7
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 1 0.00905157 0.009052 131892.6 <.0001
Error 5 0.00000034 6.863e-8
C. Total 6 0.00905191
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.008102 0.00013 0.00777 0.00844
Cold Chem 0 . . . .
Peroxide Fusions 3 0.080767 0.00015 0.08038 0.08116
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.008102 0.000074 3.71e-5 0.00798 0.00822
Cold Chem 0 . . . . .
Peroxide Fusions 3 0.080767 0.000404 0.00023 0.07976 0.08177
Tests that the Variances are Equal
0
0.0001
0.0002
0.0003
0.0004
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0000741 0.0000525 0.0000525
Cold Chem 0 . 0.0000000 0.0000000
Peroxide Fusions 3 0.0004041 0.0003111 0.0002333
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 2.3670 1 5 0.1845
Brown-Forsythe 0.8409 1 5 0.4012
Levene 13.7319 1 5 0.0139
Bartlett 4.8239 1 . 0.0281
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
94595.678 1 2.1012 <.0001
Oneway Analysis of Ca By Prep Grouping=SB7b SRAT, Type=Receipt
0.6
0.65
0.7
0.75
Ca
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.865427
Adj Rsquare 0.831784
Root Mean Square Error 0.021864
Mean of Response 0.677909
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.02459449 0.012297 25.7237 0.0003
Error 8 0.00382442 0.000478
C. Total 10 0.02841891
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.637750 0.01093 0.61254 0.66296
Cold Chem 4 0.661500 0.01093 0.63629 0.68671
Peroxide Fusions 3 0.753333 0.01262 0.72422 0.78244
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.637750 0.030126 0.01506 0.58981 0.68569
Cold Chem 4 0.661500 0.011387 0.00569 0.64338 0.67962
Peroxide Fusions 3 0.753333 0.018877 0.01090 0.70644 0.80023
Tests that the Variances are Equal
0.000
0.010
0.020
0.030
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
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Fu
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ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0301261 0.0227500 0.0227500
Cold Chem 4 0.0113871 0.0082500 0.0070000
Peroxide Fusions 3 0.0188768 0.0137778 0.0163333
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 1.1041 2 8 0.3772
Brown-Forsythe 1.5656 2 8 0.2668
Levene 1.8718 2 8 0.2154
Bartlett 1.0986 2 . 0.3333
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
27.3596 2 4.2734 0.0037
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Peroxide Fusions A 0.75333333
Cold Chem B 0.66150000
Aqua Regia B 0.63775000
Levels not connected by same letter are significantly different.
SRNL-STI-2011-00475, REVISION 0
54
Oneway Analysis of Cr By Prep Grouping=SB7b SRAT, Type=Receipt
0.04
0.045
0.05
0.055
0.06
0.065
0.07
0.075
Cr
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.610576
Adj Rsquare 0.51322
Root Mean Square Error 0.00696
Mean of Response 0.048264
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.00060762 0.000304 6.2716 0.0230
Error 8 0.00038754 0.000048
C. Total 10 0.00099517
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.043075 0.00348 0.03505 0.05110
Cold Chem 4 0.044375 0.00348 0.03635 0.05240
Peroxide Fusions 3 0.060367 0.00402 0.05110 0.06963
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.043075 0.002498 0.00125 0.03910 0.04705
Cold Chem 4 0.044375 0.001144 0.00057 0.04255 0.04620
Peroxide Fusions 3 0.060367 0.013507 0.00780 0.02681 0.09392
Tests that the Variances are Equal
0.000
0.004
0.008
0.012
0.016
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0024985 0.0019750 0.0019750
Cold Chem 4 0.0011442 0.0007250 0.0007250
Peroxide Fusions 3 0.0135072 0.0101111 0.0107333
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 2.4783 2 8 0.1453
Brown-Forsythe 6.3180 2 8 0.0226
Levene 10.8086 2 8 0.0053
Bartlett 6.1042 2 . 0.0022
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
2.1970 2 3.6319 0.2370
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Peroxide Fusions A 0.06036667
Cold Chem B 0.04437500
Aqua Regia B 0.04307500
Levels not connected by same letter are significantly different.
Oneway Analysis of Cu By Prep Grouping=SB7b SRAT, Type=Receipt
0.04
0.045
0.05
0.055
0.06
0.065
0.07
0.075
0.08
0.085
Cu
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.977384
Adj Rsquare 0.97173
Root Mean Square Error 0.002912
Mean of Response 0.058518
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.00293150 0.001466 172.8629 <.0001
Error 8 0.00006783 8.479e-6
C. Total 10 0.00299934
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.080000 0.00146 0.07664 0.08336
Cold Chem 4 0.044425 0.00146 0.04107 0.04778
Peroxide Fusions 3 0.048667 0.00168 0.04479 0.05254
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.080000 0.004190 0.00209 0.07333 0.08667
Cold Chem 4 0.044425 0.000299 0.00015 0.04395 0.04490
Peroxide Fusions 3 0.048667 0.002730 0.00158 0.04188 0.05545
Tests that the Variances are Equal
0
0.001
0.002
0.003
0.004
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0041897 0.0032000 0.0032000
Cold Chem 4 0.0002986 0.0002250 0.0002250
Peroxide Fusions 3 0.0027301 0.0020889 0.0018667
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 1.5275 2 8 0.2742
Brown-Forsythe 2.7520 2 8 0.1232
Levene 5.3045 2 8 0.0342
Bartlett 5.0015 2 . 0.0067
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
121.7612 2 3.2471 0.0009
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Aqua Regia A 0.08000000
Peroxide Fusions B 0.04866667
Cold Chem B 0.04442500
Levels not connected by same letter are significantly different.
SRNL-STI-2011-00475, REVISION 0
55
Oneway Analysis of Fe By Prep Grouping=SB7b SRAT, Type=Receipt
13.5
14
14.5
15
Fe
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.095539
Adj Rsquare -0.13058
Root Mean Square Error 0.392906
Mean of Response 14.33636
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.1304545 0.065227 0.4225 0.6692
Error 8 1.2350000 0.154375
C. Total 10 1.3654545
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 14.2250 0.19645 13.772 14.678
Cold Chem 4 14.4750 0.19645 14.022 14.928
Peroxide Fusions 3 14.3000 0.22684 13.777 14.823
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 14.2250 0.639661 0.31983 13.207 15.243
Cold Chem 4 14.4750 0.050000 0.02500 14.395 14.555
Peroxide Fusions 3 14.3000 2.18e-15 1.3e-15 14.300 14.300
Tests that the Variances are Equal
0.0
0.2
0.4
0.6
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.6396614 0.4750000 0.4750000
Cold Chem 4 0.0500000 0.0375000 0.0250000
Peroxide Fusions 3 2.176e-15 1.776e-15 0.0000000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 1.9155 2 8 0.2091
Brown-Forsythe 4.7592 2 8 0.0435
Levene 6.4377 2 8 0.0216
Bartlett 59.9663 2 . <.0001
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
21.0236 2 4 0.0075
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Cold Chem A 14.475000
Peroxide Fusions A 14.300000
Aqua Regia A 14.225000
Levels not connected by same letter are significantly different.
Oneway Analysis of K By Prep Grouping=SB7b SRAT, Type=Receipt
0
0.05
0.1
0.15
0.2
0.25
K
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.999945
Adj Rsquare 0.999931
Root Mean Square Error 0.000833
Mean of Response 0.1474
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.10096466 0.050482 72680.02 <.0001
Error 8 0.00000556 6.946e-7
C. Total 10 0.10097022
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.025600 0.00042 0.02464 0.02656
Cold Chem 4 0.188250 0.00042 0.18729 0.18921
Peroxide Fusions 3 0.255333 0.00048 0.25422 0.25644
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.025600 0.000216 0.00011 0.02526 0.02594
Cold Chem 4 0.188250 0.000957 0.00048 0.18673 0.18977
Peroxide Fusions 3 0.255333 0.001155 0.00067 0.25246 0.25820
Tests that the Variances are Equal
0
0.0004
0.0008
0.0012
Std
Dev
Aq
ua R
eg
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Co
ld C
hem
Pero
xid
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Fu
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ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0002160 0.0001500 0.0001500
Cold Chem 4 0.0009574 0.0007500 0.0007500
Peroxide Fusions 3 0.0011547 0.0008889 0.0006667
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 1.3300 2 8 0.3172
Brown-Forsythe 0.9462 2 8 0.4277
Levene 5.3895 2 8 0.0329
Bartlett 2.5410 2 . 0.0788
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
91164.396 2 3.4179 <.0001
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Peroxide Fusions A 0.25533333
Cold Chem B 0.18825000
Aqua Regia C 0.02560000
Levels not connected by same letter are significantly different.
SRNL-STI-2011-00475, REVISION 0
56
Oneway Analysis of Li By Prep Grouping=SB7b SRAT, Type=Receipt
0.023
0.024
0.025
0.026
0.027
0.028
Li
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.673347
Adj Rsquare 0.591684
Root Mean Square Error 0.000984
Mean of Response 0.0251
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.00001596 7.9792e-6 8.2454 0.0114
Error 8 0.00000774 9.6771e-7
C. Total 10 0.00002370
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.026475 0.00049 0.02534 0.02761
Cold Chem 4 0.024975 0.00049 0.02384 0.02611
Peroxide Fusions 3 0.023433 0.00057 0.02212 0.02474
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.026475 0.001473 0.00074 0.02413 0.02882
Cold Chem 4 0.024975 0.000427 0.00021 0.02430 0.02565
Peroxide Fusions 3 0.023433 0.000586 0.00034 0.02198 0.02489
Tests that the Variances are Equal
0
0.0005
0.001
0.0015
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
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Fu
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ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0014728 0.0011250 0.0011250
Cold Chem 4 0.0004272 0.0003250 0.0003250
Peroxide Fusions 3 0.0005859 0.0004444 0.0004333
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 1.6860 2 8 0.2449
Brown-Forsythe 2.2361 2 8 0.1693
Levene 3.4896 2 8 0.0814
Bartlett 1.9834 2 . 0.1376
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
9.3019 2 4.4504 0.0257
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Aqua Regia A 0.02647500
Cold Chem A B 0.02497500
Peroxide Fusions B 0.02343333
Levels not connected by same letter are significantly different.
Oneway Analysis of Mg By Prep Grouping=SB7b SRAT, Type=Receipt
0.265
0.27
0.275
0.28
0.285
0.29
0.295
0.3
Mg
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.518046
Adj Rsquare 0.397557
Root Mean Square Error 0.008526
Mean of Response 0.286636
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.00062505 0.000313 4.2995 0.0540
Error 8 0.00058150 0.000073
C. Total 10 0.00120655
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.284750 0.00426 0.27492 0.29458
Cold Chem 4 0.295750 0.00426 0.28592 0.30558
Peroxide Fusions 3 0.277000 0.00492 0.26565 0.28835
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.284750 0.013720 0.00686 0.26292 0.30658
Cold Chem 4 0.295750 0.000957 0.00048 0.29423 0.29727
Peroxide Fusions 3 0.277000 0.002646 0.00153 0.27043 0.28357
Tests that the Variances are Equal
0.000
0.004
0.008
0.012
0.016
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
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Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0137204 0.0102500 0.0102500
Cold Chem 4 0.0009574 0.0007500 0.0007500
Peroxide Fusions 3 0.0026458 0.0020000 0.0020000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 1.8963 2 8 0.2118
Brown-Forsythe 3.7088 2 8 0.0725
Levene 5.6388 2 8 0.0297
Bartlett 6.3672 2 . 0.0017
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
58.5623 2 3.5639 0.0019
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Cold Chem A 0.29575000
Aqua Regia A B 0.28475000
Peroxide Fusions B 0.27700000
Levels not connected by same letter are significantly different.
SRNL-STI-2011-00475, REVISION 0
57
Oneway Analysis of Mn By Prep Grouping=SB7b SRAT, Type=Receipt
2.8
2.85
2.9
2.95
3
3.05
3.1
3.15
Mn
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.388701
Adj Rsquare 0.235877
Root Mean Square Error 0.089005
Mean of Response 3.044545
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.04029773 0.020149 2.5434 0.1396
Error 8 0.06337500 0.007922
C. Total 10 0.10367273
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 3.01500 0.04450 2.9124 3.1176
Cold Chem 4 3.12250 0.04450 3.0199 3.2251
Peroxide Fusions 3 2.98000 0.05139 2.8615 3.0985
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 3.01500 0.144799 0.07240 2.7846 3.2454
Cold Chem 4 3.12250 0.009574 0.00479 3.1073 3.1377
Peroxide Fusions 3 2.98000 0.010000 0.00577 2.9552 3.0048
Tests that the Variances are Equal
0.00
0.05
0.10
0.15
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
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Fu
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ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.1447987 0.1100000 0.1100000
Cold Chem 4 0.0095743 0.0075000 0.0075000
Peroxide Fusions 3 0.0100000 0.0066667 0.0100000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 2.1186 2 8 0.1827
Brown-Forsythe 4.9960 2 8 0.0391
Levene 7.3700 2 8 0.0153
Bartlett 8.1808 2 . 0.0003
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
158.4136 2 4.7318 <.0001
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Cold Chem A 3.1225000
Aqua Regia A 3.0150000
Peroxide Fusions A 2.9800000
Levels not connected by same letter are significantly different.
Oneway Analysis of Na By Prep Grouping=SB7b SRAT, Type=Receipt
13.5
14
14.5
15
Na
Aq
ua R
eg
ia
Co
ld C
hem
Prep
Missing Rows 3
Oneway Anova
Summary of Fit
Rsquare 0.246951
Adj Rsquare 0.121443
Root Mean Square Error 0.453689
Mean of Response 14.35
Observations (or Sum Wgts) 8
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 1 0.4050000 0.405000 1.9676 0.2103
Error 6 1.2350000 0.205833
C. Total 7 1.6400000
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 14.1250 0.22684 13.570 14.680
Cold Chem 4 14.5750 0.22684 14.020 15.130
Peroxide Fusions 0 . . . .
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 14.1250 0.639661 0.31983 13.107 15.143
Cold Chem 4 14.5750 0.050000 0.02500 14.495 14.655
Peroxide Fusions 0 . . . . .
Tests that the Variances are Equal
0.0
0.2
0.4
0.6
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.6396614 0.4750000 0.4750000
Cold Chem 4 0.0500000 0.0375000 0.0250000
Peroxide Fusions 0 . 0.0000000 0.0000000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 2.2457 1 6 0.1846
Brown-Forsythe 5.3407 1 6 0.0602
Levene 7.0268 1 6 0.0380
Bartlett 9.5753 1 . 0.0020
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
1.9676 1 3.0367 0.2542
SRNL-STI-2011-00475, REVISION 0
58
Oneway Analysis of Ni By Prep Grouping=SB7b SRAT, Type=Receipt
2.8
2.85
2.9
2.95
3
3.05
3.1
3.15
Ni
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
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Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.054643
Adj Rsquare -0.1817
Root Mean Square Error 0.083267
Mean of Response 2.954545
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.00320606 0.001603 0.2312 0.7987
Error 8 0.05546667 0.006933
C. Total 10 0.05867273
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 2.93500 0.04163 2.8390 3.0310
Cold Chem 4 2.97500 0.04163 2.8790 3.0710
Peroxide Fusions 3 2.95333 0.04807 2.8425 3.0642
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 2.93500 0.135277 0.06764 2.7197 3.1503
Cold Chem 4 2.97500 0.010000 0.00500 2.9591 2.9909
Peroxide Fusions 3 2.95333 0.011547 0.00667 2.9246 2.9820
Tests that the Variances are Equal
0.00
0.04
0.08
0.12
0.16
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
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Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.1352775 0.1000000 0.1000000
Cold Chem 4 0.0100000 0.0075000 0.0050000
Peroxide Fusions 3 0.0115470 0.0088889 0.0066667
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 1.8793 2 8 0.2143
Brown-Forsythe 4.4452 2 8 0.0503
Levene 5.7325 2 8 0.0285
Bartlett 7.5441 2 . 0.0005
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
3.0503 2 4.5949 0.1435
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Cold Chem A 2.9750000
Peroxide Fusions A 2.9533333
Aqua Regia A 2.9350000
Levels not connected by same letter are significantly different.
Oneway Analysis of Si By Prep Grouping=SB7b SRAT, Type=Receipt
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1
1.1
Si
Aq
ua R
eg
ia
Pero
xid
e
Fu
sio
ns
Prep
Missing Rows 4
Oneway Anova
Summary of Fit
Rsquare 0.962297
Adj Rsquare 0.954756
Root Mean Square Error 0.067793
Mean of Response 0.722429
Observations (or Sum Wgts) 7
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 1 0.58650430 0.586504 127.6151 <.0001
Error 5 0.02297942 0.004596
C. Total 6 0.60948371
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.47175 0.03390 0.38462 0.5589
Cold Chem 0 . . . .
Peroxide Fusions 3 1.05667 0.03914 0.95605 1.1573
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.47175 0.087393 0.04370 0.3327 0.6108
Cold Chem 0 . . . . .
Peroxide Fusions 3 1.05667 0.005774 0.00333 1.0423 1.0710
Tests that the Variances are Equal
0.00
0.02
0.04
0.06
0.08
0.10
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0873933 0.0602500 0.0602500
Cold Chem 0 . 0.0000000 0.0000000
Peroxide Fusions 3 0.0057735 0.0044444 0.0033333
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 1.4622 1 5 0.2806
Brown-Forsythe 3.2747 1 5 0.1301
Levene 3.1779 1 5 0.1347
Bartlett 6.8771 1 . 0.0087
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
178.1444 1 3.0349 0.0009
SRNL-STI-2011-00475, REVISION 0
59
Oneway Analysis of Th By Prep Grouping=SB7b SRAT, Type=Receipt
0.7
0.8
0.9
1
1.1
Th
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.863068
Adj Rsquare 0.828835
Root Mean Square Error 0.056129
Mean of Response 0.914182
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.15885422 0.079427 25.2115 0.0004
Error 8 0.02520342 0.003150
C. Total 10 0.18405764
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 1.03600 0.02806 0.97128 1.1007
Cold Chem 4 0.76075 0.02806 0.69603 0.8255
Peroxide Fusions 3 0.95633 0.03241 0.88161 1.0311
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 1.03600 0.049450 0.02473 0.95731 1.1147
Cold Chem 4 0.76075 0.073082 0.03654 0.64446 0.8770
Peroxide Fusions 3 0.95633 0.030370 0.01753 0.88089 1.0318
Tests that the Variances are Equal
0.00
0.02
0.04
0.06
0.08
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
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Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0494503 0.0390000 0.0390000
Cold Chem 4 0.0730816 0.0552500 0.0552500
Peroxide Fusions 3 0.0303699 0.0224444 0.0253333
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 0.9312 2 8 0.4329
Brown-Forsythe 1.0278 2 8 0.4006
Levene 1.3762 2 8 0.3064
Bartlett 0.6958 2 . 0.4987
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
17.2954 2 5.2486 0.0049
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Aqua Regia A 1.0360000
Peroxide Fusions A 0.9563333
Cold Chem B 0.7607500
Levels not connected by same letter are significantly different.
Oneway Analysis of Ti By Prep Grouping=SB7b SRAT, Type=Receipt
0.015
0.016
0.017
0.018
0.019
0.02
0.021
0.022
Ti
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.66892
Adj Rsquare 0.58615
Root Mean Square Error 0.001032
Mean of Response 0.018518
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.00001720 8.6011e-6 8.0817 0.0120
Error 8 0.00000851 1.0643e-6
C. Total 10 0.00002572
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.016875 0.00052 0.01569 0.01806
Cold Chem 4 0.019300 0.00052 0.01811 0.02049
Peroxide Fusions 3 0.019667 0.00060 0.01829 0.02104
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.016875 0.000869 0.00043 0.01549 0.01826
Cold Chem 4 0.019300 0.001438 0.00072 0.01701 0.02159
Peroxide Fusions 3 0.019667 0.000153 8.82e-5 0.01929 0.02005
Tests that the Variances are Equal
0
0.0005
0.001
0.0015
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0008694 0.0006750 0.0006750
Cold Chem 4 0.0014376 0.0010500 0.0009000
Peroxide Fusions 3 0.0001528 0.0001111 0.0001333
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 0.8892 2 8 0.4480
Brown-Forsythe 0.9336 2 8 0.4321
Levene 2.6963 2 8 0.1273
Bartlett 2.8442 2 . 0.0582
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
17.1540 2 4.2116 0.0095
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Peroxide Fusions A 0.01966667
Cold Chem A 0.01930000
Aqua Regia B 0.01687500
Levels not connected by same letter are significantly different.
SRNL-STI-2011-00475, REVISION 0
60
Oneway Analysis of U By Prep Grouping=SB7b SRAT, Type=Receipt
4.4
4.5
4.6
4.7
4.8
4.9
5
5.1
U
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Oneway Anova
Summary of Fit
Rsquare 0.823719
Adj Rsquare 0.779649
Root Mean Square Error 0.112884
Mean of Response 4.760909
Observations (or Sum Wgts) 11
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 2 0.47634924 0.238175 18.6911 0.0010
Error 8 0.10194167 0.012743
C. Total 10 0.57829091
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 4.77250 0.05644 4.6423 4.9027
Cold Chem 4 4.98000 0.05644 4.8498 5.1102
Peroxide Fusions 3 4.45333 0.06517 4.3030 4.6036
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 4.77250 0.175950 0.08797 4.4925 5.0525
Cold Chem 4 4.98000 0.028284 0.01414 4.9350 5.0250
Peroxide Fusions 3 4.45333 0.057735 0.03333 4.3099 4.5968
Tests that the Variances are Equal
0.00
0.05
0.10
0.15
0.20
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.1759498 0.1425000 0.1425000
Cold Chem 4 0.0282843 0.0200000 0.0200000
Peroxide Fusions 3 0.0577350 0.0444444 0.0333333
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 3.2165 2 8 0.0944
Brown-Forsythe 6.9551 2 8 0.0178
Levene 9.9973 2 8 0.0067
Bartlett 3.5460 2 . 0.0288
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
91.0739 2 3.8604 0.0006
Means Comparisons
Comparisons for all pairs using Tukey-Kramer HSD
Level Mean
Cold Chem A 4.9800000
Aqua Regia A 4.7725000
Peroxide Fusions B 4.4533333
Levels not connected by same letter are significantly different.
Oneway Analysis of Zr By Prep Grouping=SB7b SRAT, Type=Receipt
0.1
0.15
0.2
0.25
Zr
Aq
ua R
eg
ia
Co
ld C
hem
Prep
Missing Rows 3
Oneway Anova
Summary of Fit
Rsquare 0.951867
Adj Rsquare 0.943845
Root Mean Square Error 0.01691
Mean of Response 0.204375
Observations (or Sum Wgts) 8
Analysis of Variance
Source DF Sum of Squares Mean Square F Ratio Prob > F
Prep 1 0.03393013 0.033930 118.6541 <.0001
Error 6 0.00171575 0.000286
C. Total 7 0.03564588
Means for Oneway Anova
Level Number Mean Std Error Lower 95% Upper 95%
Aqua Regia 4 0.139250 0.00846 0.11856 0.15994
Cold Chem 4 0.269500 0.00846 0.24881 0.29019
Peroxide Fusions 0 . . . .
Std Error uses a pooled estimate of error variance
Means and Std Deviations
Level Number Mean Std Dev Std Err Mean Lower 95% Upper 95%
Aqua Regia 4 0.139250 0.023796 0.01190 0.10139 0.17711
Cold Chem 4 0.269500 0.002380 0.00119 0.26571 0.27329
Peroxide Fusions 0 . . . . .
Tests that the Variances are Equal
0.000
0.005
0.010
0.015
0.020
0.025
Std
Dev
Aq
ua R
eg
ia
Co
ld C
hem
Pero
xid
e
Fu
sio
ns
Prep
Level Count Std Dev MeanAbsDif to Mean MeanAbsDif to Median
Aqua Regia 4 0.0237960 0.0182500 0.0182500
Cold Chem 4 0.0023805 0.0020000 0.0020000
Peroxide Fusions 0 . 0.0000000 0.0000000
Test F Ratio DFNum DFDen Prob > F
O'Brien[.5] 2.6050 1 6 0.1577
Brown-Forsythe 6.0501 1 6 0.0491
Levene 8.6224 1 6 0.0261
Bartlett 8.3264 1 . 0.0039
Warning: Small sample sizes. Use Caution.
Welch Anova testing Means Equal, allowing Std Devs Not Equal
F Ratio DFNum DFDen Prob > F
118.6541 1 3.06 0.0015
SRNL-STI-2011-00475, REVISION 0
61
Distribution
M.J. Barnes, 773-A
J.M. Bricker, 704-27S
C.J. Coleman, 773-A
T.B. Edwards, 773-42A
M.T. Feller, 704-28S
T.L. Fellinger, 704-26S
C.M. Gregory, 773-A
C.C. Herman, 999-W
E.W. Holtzscheiter, 704-15S
J.F. Iaukea, 704-30S
P.L. Lee, 773-A
S.L. Marra, 773-A
R.T. McNew, 704-S
R.N. Mahannah, 704-28S
A.B. Osteen, 704-28S
J.E. Occhipinti, 704-S
J.M. Pareizs, 773-A
D.K. Peeler, 999-W
H.M. Pittman, 704-27S
J.W. Ray, 704-S
D.C. Sherburne, 704-S
A.V. Staub, 704-27S
M.E. Stone, 999-W
B.J. Wiedenman, 773-A